CN116273102B - Laminated composite photocatalyst with mesoporous film and preparation method and application thereof - Google Patents
Laminated composite photocatalyst with mesoporous film and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011159 matrix material Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002135 nanosheet Substances 0.000 claims description 19
- 238000005303 weighing Methods 0.000 claims description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 125000000542 sulfonic acid group Chemical group 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 12
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 11
- 239000012467 final product Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229960003638 dopamine Drugs 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
- 238000011161 development Methods 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000002064 nanoplatelet Substances 0.000 description 4
- 238000006303 photolysis reaction Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910002915 BiVO4 Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000004098 Tetracycline Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000004298 light response Effects 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 229960002180 tetracycline Drugs 0.000 description 3
- 229930101283 tetracycline Natural products 0.000 description 3
- 235000019364 tetracycline Nutrition 0.000 description 3
- 150000003522 tetracyclines Chemical class 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000001841 imino group Chemical group [H]N=* 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
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- 239000002114 nanocomposite Substances 0.000 description 2
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- 230000008569 process Effects 0.000 description 2
- 210000002966 serum Anatomy 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000010523 cascade reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical group OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 239000011206 ternary composite Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
-
- 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
-
- 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 & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a laminated composite photocatalyst with a mesoporous film, a preparation method and application thereof, wherein the composite photocatalyst consists of a carrier matrix, a surface coating and a binder, and has a laminated structure; the carrier matrix accounts for 68.0-99.0% of the weight of the composite photocatalyst, the surface coating accounts for 0.5-30.0% of the weight of the composite photocatalyst, and the binder accounts for 0.5-2.0% of the weight of the composite photocatalyst; can be used for decomposing water into hydrogen by photocatalysis. The laminated composite photocatalyst with the mesoporous film has high activity, good stability and low cost, is suitable for the reaction of decomposing water into hydrogen by photocatalysis, and has high hydrogen yield.
Description
Technical Field
The invention relates to the technical field of photocatalysts and preparation thereof, in particular to a laminated composite photocatalyst with mesoporous membrane, and a preparation method and application thereof.
Background
Compared to traditional fossil energy sources, hydrogen energy is gaining attention for its efficiency and cleanliness. The scientists in all countries compete for developing technologies and products related to hydrogen energy, and the low-cost hydrogen can be obtained quickly and efficiently, so that the hydrogen energy economy can be achieved. The traditional hydrogen production mode mainly generates hydrogen through the pyrolysis of coal, petroleum and natural gas; or hydrogen is produced by electrolysis of water; since a large amount of fossil fuel is consumed in the process of hydrogen production and causes regional environmental pollution and global warming, development of a green clean hydrogen production pathway is one of targets for hydrogen energy development.
Solar energy and water are two important renewable resources on earth, and the use of solar energy to decompose water to produce hydrogen is the cleanest hydrogen production route, and has been a dream for human development of hydrogen energy. Therefore, the research of a novel photocatalyst for producing hydrogen by photolysis of water is a future development direction. Bismuth vanadate (BiVO 4) is considered as one of the most promising photoanode materials for producing hydrogen by photodecomposition of water. BiVO4 has a bandgap of 2.4 eV, and a theoretical photocurrent density of 7.5 mA/cm 2 at an illuminance of AM 1.5G (100 mW/cm 2) with a corresponding Solar To Hydrogen (STH) efficiency of 9.2%. Although the band gap of BiVO 4 is slightly larger than the ideal band gap of 2.0 eV for photodecomposition of water, its conduction band edge is located very close to the H 2 precipitation potential, so in the low potential region, biVO 4 has a lower onset potential and higher photocurrent density than many other photoanode materials. Researchers in the university of osaka in japan compound Black Phosphorus (BP) and BiVO 4 with a two-dimensional structure to prepare a brand new two-dimensional BP/BiVO 4 compound heterojunction catalyst, which has a broad spectral response range from ultraviolet to visible light and excellent electron-hole separation performance, and can obtain excellent hydrogen production efficiency by photolysis without sacrificing agent and additional energy consumption. In addition, researchers at Tianjin university controllably introduce oxygen vacancies on the surface of the BiVO 4 photo-anode by a photo-etching method, so that the photo-electric activity of BiVO 4 is greatly improved, and after the thickness of the BiVO 4 electrode is optimized and the auxiliary agent is loaded, The high-efficiency bias-free self-water-dissolving device is obtained by connecting the high-efficiency bias-free self-water-dissolving device with a silicon cathode in series, and the solar energy conversion efficiency is as high as 3.5%.
CN201710351559 discloses a construction method of a photoelectrochemical sensor for enzyme-free detection of dopamine, in the patent, a photoelectrochemical sensing platform is successfully built by preparing a nano-composite of BiOCl/BiVO 4/aza graphene quantum dots (N-GQDs) as a photoelectroactive material, and the properties of the nano-composite of BiOCl/BiVO 4/N-GQDs, such as larger absorption and quick response of visible light, are utilized to play a role in signal amplification for a detection system. The method is used for enzyme-free photoelectrochemical detection of dopamine in human serum, a photoelectrochemical sensor for rapidly and sensitively detecting the dopamine is constructed, a corresponding relation between the concentration of the dopamine and a photocurrent response value is established, and the purpose of simply, sensitively and rapidly detecting the dopamine is realized. Thus, the prepared sensor can be used for detecting the dopamine content in human serum.
CN201811361797 discloses a preparation method of visible light responsive Fe 3O4 quantum dot modified BiOCl/BiVO 4, a visible light responsive Fe 3O4 quantum dot modified BiOCl/BiVO 4 composite photocatalyst is obtained, a simple and rapid method is utilized to prepare a Fe 3O4 quantum dot modified BiOCl/BiVO 4 p-n heterojunction, excellent photocatalytic activity is shown when various antibiotics are degraded under visible light, and a sample has stronger magnetism and is easy to recycle.
CN202010215888.6 discloses a method for preparing a carbon cloth supported BiOCl/BiVO 4 recyclable flexible composite photocatalytic material and application thereof, the carbon cloth supported BiOCl/BiVO4 recyclable flexible composite photocatalytic material takes simple and easy-to-obtain carbon cloth as a substrate, has excellent conductivity, flexibility and bendability, can be cut according to different use environments without worrying about material damage even if being folded or repeatedly bent for a long time, has the advantages of high carrier diffusion rate, wide light response range, recycling, good cycle performance and low cost, improves the defects of little BiOCl light absorption and large energy loss, and solves the problems of difficult separation and recycling of a powder photocatalyst, thereby realizing sustainable development and recycling of resources.
CN202110064257.3 discloses a modified diatomite-supported BiVO 4 -BiOCl heterojunction composite material, rich amino groups and imino groups are introduced on the surface of diatomite, a large number of amino groups and imino groups can be used as active adsorption sites, so that the modified diatomite can effectively adsorb pollutants such as tetracycline through the actions of hydrogen bond association, electrostatic action and the like, the functional modification of the diatomite is realized, p-n heterojunction is formed by BiOCl nanoflower and Zn-doped mesoporous BiVO4, separation of photo-generated electrons and holes is promoted, active substances such as hydroxyl free radicals and superoxide free radicals are further generated by reaction with water, firstly, the modified diatomite effectively adsorbs the tetracycline through hydrogen bond association and electrostatic action, and then is photo-catalytically degraded into nontoxic small molecules, and therefore the high-efficiency adsorption and photo-catalytic degradation processes of the tetracycline are realized.
Although the photocatalysts belong to composite photocatalysts, the photocatalysts respectively construct ternary composite photocatalysts by using aza graphene quantum dots, fe 3O4 quantum dots, carbon cloth and modified diatomite and BiVO 4 -BiOCl heterojunction, wherein the aza graphene quantum dots, fe 3O4 quantum dots and carbon cloth can enhance conductivity, and the modified diatomite can enhance adsorption, so that the performances are single and the cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a laminated composite photocatalyst with mesoporous membrane, which has high activity, good stability and low cost, and is suitable for the reaction of photocatalytic decomposition of water to produce hydrogen, and a preparation method and application thereof.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
A first object of the present invention is to provide a laminated composite photocatalyst having a mesoporous film, the composite photocatalyst being composed of a support matrix, a surface coating layer and a binder, and having a laminated structure; the carrier matrix accounts for 68.0-99.0% of the weight of the composite photocatalyst, the surface coating accounts for 0.5-30.0% of the weight of the composite photocatalyst, and the binder accounts for 0.5-2.0% of the weight of the composite photocatalyst.
Preferably, the carrier matrix accounts for 84.0-94.5% of the weight of the composite photocatalyst, the surface coating accounts for 5.0-15.0% of the weight of the composite photocatalyst, and the binder accounts for 0.5-1.0% of the weight of the composite photocatalyst.
Preferably, the carrier matrix is a layered Ti 3C2 nanometer sheet, and the thickness of a single sheet layer in the layered structure of the layered Ti 3C2 nanometer sheet is 1-200 nm.
Preferably, the surface coating is a mesoporous film, and the aperture of the mesoporous film is 2-40 nm.
Preferably, the binder is a perfluorosulfonic acid resin.
A first object of the present invention is to provide a method for preparing a laminated composite photocatalyst having a mesoporous film, comprising the steps of:
(1) Adding 40-60% hydrofluoric acid of 40-100 mL into a plastic beaker, weighing 5-10 g Ti 3AlC2, mixing with the hydrofluoric acid, stirring the mixed solution for uniform mixing for 20-60 min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifuging, treating the solution at 80-160 ℃ by using a vacuum drying box, and finally cooling the material to obtain the carrier matrix layered Ti 3C2 nano-sheet.
(2) Weighing 9-40 mg Bi (NO 3)3•5H2 O is dissolved in 10-60 mL concentration 1-4 mol/L dilute nitric acid, then 2-18 mg ammonium vanadate is added, room temperature magnetic stirring is carried out, 10-60 min is carried out, the pH value range of a solution system is regulated to 3-6 by using dilute hydrochloric acid, then 100 mg is weighed, the carrier substrate layered Ti 3C2 nano-sheets obtained in the step (1) are added with adhesive, then stirring is continued, after stirring, the liquid is transferred to a reaction kettle, 100-180 ℃ is reacted for 12-48 h, then the material is cooled at room temperature, distilled water and ethanol are respectively used for washing for two-three times, then the obtained product is placed in a vacuum drying box, the temperature is regulated to 60-120 ℃ and dried under vacuum condition for 8-24 h, finally, the obtained powder is transferred to a tubular furnace, and calcined for 6-12 h under the protection of argon gas, thus obtaining the laminated composite photocatalyst with a porous membrane.
The third object of the invention is to provide an application of the laminated composite photocatalyst with the mesoporous film in photocatalytic decomposition of water to produce hydrogen.
The photocatalysis principle of the laminated composite photocatalyst with mesoporous film of the invention is as follows: the mesoporous film has an open structure, high specific surface, excellent conductivity and visible light response, generates more high-energy electrons capable of participating in chemical reaction through light irradiation, and meanwhile, the mesoporous film structure has a large number of intimate heterojunction to effectively inhibit the recombination of photo-generated electrons and holes, so that the photocatalysis efficiency is improved.
Compared with the prior art, the mesoporous laminated composite photocatalyst with strong electric conduction and hydrophilicity is prepared, wherein a carrier matrix Ti 3C2 and a binder perfluorinated sulfonic acid resin have extremely strong electric conduction and good hydrophilicity, and in addition, the active components of the photocatalyst are BiVO 4 and BiOCl nano particles, and a film is formed on the surface of each layer of Ti 3C2 to form a laminated structure. The rich pore canal structure is beneficial to the occurrence of cascade reaction, and the active site of the photocatalytic reaction in the pore canal is increased, so that the photocatalytic efficiency is improved. And the porous open structure is beneficial to the transmission of reactants, and can also improve the photocatalysis efficiency. In addition, the mesoporous film laminated structure composite photocatalyst is not a simple superposition of original performances, but a new material with an open structure, hydrophilicity, high conductivity and visible light response, so that the photoelectric performance of the catalyst is changed in quality, and the catalyst has new functional characteristics.
Drawings
FIG. 1 is an SEM photograph of layered Ti 3C2 nanoplatelets of a support matrix prepared according to one embodiment of the present invention.
Figure 2 is an XRD spectrum of layered Ti 3C2 nanoplatelets prepared according to one embodiment of the present invention.
Figure 3 is an XRD spectrum of a composite photocatalyst prepared according to one embodiment of the present invention.
Fig. 4 is an SEM photograph of a composite photocatalyst prepared according to an embodiment of the present invention.
Fig. 5 is a TEM photograph of a composite photocatalyst prepared according to one embodiment of the present invention.
FIG. 6 is a graph showing pore size distribution of a composite photocatalyst prepared according to an embodiment of the present invention.
Description of the embodiments
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. The specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
The materials and reagents used in the following examples are commercially available except for the specific descriptions, and the specific sources thereof are not described in detail in the following examples.
Example 1
(1) Weighing 10 g Ti 3AlC2 materials, adding 100 mL of 50% hydrofluoric acid, uniformly mixing, stirring the mixed solution for 60: 60min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifugally separating, treating at 120 ℃ by using a vacuum drying oven, and finally cooling the materials to obtain the carrier matrix layered Ti 3C2 nano-sheets.
(2) 9.7 Mg Bi (NO 3)3•5H2 O is dissolved in dilute nitric acid with the concentration of 20 mL and 2 mol/L, 2.3 mg NH 4VO3 is added, the pH value range of a solution system is regulated to 5 by using dilute hydrochloric acid under room temperature magnetic stirring, 100 mg layered Ti 3C2 nano sheets of the carrier matrix obtained in the step (1) are weighed, 1 mu L of binder is added, stirring is continued for 30 min, liquid is transferred to a reaction kettle after stirring is finished, the reaction is carried out at 160 ℃ for 24h, then the material is cooled under room temperature, distilled water and ethanol are respectively used for washing for two to three times after the material is cooled, then the obtained product is placed in a vacuum drying box, the temperature is regulated to 120 ℃ and the obtained product is dried under vacuum for 12h under the condition, finally, the obtained powder is transferred to a tubular furnace, and the obtained powder is calcined for 8h under the protection of argon gas at 400 ℃ to obtain the final product A.
Example 2
(1) Weighing 10 g Ti 3AlC2 materials, adding 100 mL of 50% hydrofluoric acid, uniformly mixing, stirring the mixed solution for 60: 60min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifugally separating, treating at 120 ℃ by using a vacuum drying oven, and finally cooling the materials to obtain the carrier matrix layered Ti 3C2 nano-sheets.
(2) The preparation method comprises the steps of weighing 100 mg layered Ti 3C2 nano-sheets of the carrier substrate obtained in the step (1), dispersing the layered Ti 3C2 nano-sheets into 10mL absolute ethanol solution, carrying out ultrasonic dispersion for 30min, then weighing 19.4 mg Bi (NO 3)3•5H2 O is dissolved in dilute nitric acid with the concentration of 20 mol/L, then adding 4.6 mg NH 4VO3, magnetically stirring at room temperature for 60 min, regulating the pH value of a solution system to be 5 by using dilute hydrochloric acid, weighing 1.2 mu L of the adhesive and then continuing stirring for 30min, transferring the liquid to a reaction kettle after stirring is finished, reacting for 24h at 160 ℃, then cooling the material at room temperature, washing the material for two to three times by using distilled water, then placing the obtained product into a vacuum drying box, regulating the temperature to 120 ℃ and drying under vacuum for 12 h, finally transferring the obtained powder into a tubular furnace, and calcining the obtained powder at the temperature of h ℃ under the protection of argon gas to obtain the final product of h B.
Example 3
(1) Weighing 10 g Ti 3AlC2 materials, adding 100 mL of 50% hydrofluoric acid, uniformly mixing, stirring the mixed solution for 60: 60min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifugally separating, treating at 120 ℃ by using a vacuum drying oven, and finally cooling the materials to obtain the carrier matrix layered Ti 3C2 nano-sheets.
(2) The preparation method comprises the steps of weighing 100 mg layered Ti 3C2 nano-sheets of the carrier substrate obtained in the step (1), dispersing the layered Ti 3C2 nano-sheets into a 10mL absolute ethanol solution, carrying out ultrasonic dispersion for 30min, then weighing 29.1 mg Bi (NO 3)3•5H2 O is dissolved in 2 mol/L dilute nitric acid with the concentration of 20mL, then adding 6.9 mg NH 4VO3, magnetically stirring for 60 min at room temperature, adjusting the pH value of a solution system to be 5 by using dilute hydrochloric acid, weighing 100 mg layered Ti 3C2 nano-sheets of the carrier substrate obtained in the step (1), adding 1.4 mu L of a binder, then continuing stirring for 30min, transferring the liquid to a reaction kettle after stirring is finished, reacting for 24h at 160 ℃, then cooling the material at room temperature, then washing the material for two to three times by using distilled water, then placing the obtained product in a vacuum drying box, adjusting the temperature to 120 ℃ and drying for 12 h under the vacuum condition, finally transferring the obtained powder to a tube furnace, and calcining for 8C under the protection of h ℃ under the argon.
Example 4
(1) Weighing 10 g Ti 3AlC2 materials, adding 100 mL of 50% hydrofluoric acid, uniformly mixing, stirring the mixed solution for 60: 60min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifugally separating, treating at 120 ℃ by using a vacuum drying oven, and finally cooling the materials to obtain the carrier matrix layered Ti 3C2 nano-sheets.
(2) The preparation method comprises the steps of weighing 100 mg layered Ti 3C2 nano-sheets of a carrier substrate obtained in the step (1), dispersing the layered Ti 3C2 nano-sheets into a 10mL absolute ethanol solution, carrying out ultrasonic dispersion for 30min, then weighing 38.8 mg Bi (NO 3)3•5H2 O is dissolved in dilute nitric acid with the concentration of 2 mol/L of 20mL, then adding 9.2 mg NH 4VO3, magnetically stirring at room temperature for 60 min, regulating the pH value of a solution system to be 5 by using dilute hydrochloric acid, weighing 100 mg layered Ti 3C2 nano-sheets of the carrier substrate obtained in the step (1), adding 1.6 mu L of a binder, continuing stirring for 30min, transferring the liquid to a reaction kettle after stirring is finished, reacting for 24h at 160 ℃, cooling the material at room temperature, washing the material for two to three times by using distilled water, then placing the obtained product in a vacuum drying box, regulating the temperature to 120 ℃ and drying under the vacuum condition for 12 h, finally transferring the obtained powder to a tube furnace, and calcining the obtained powder at the temperature of h ℃ under the protection of argon gas, thus obtaining the final product D at the temperature of h.
Taking the layered Ti 3C2 nano-sheets of the carrier matrix prepared in example 4 and the final product D as examples, detection was carried out.
FIG. 1 is an SEM photograph of layered Ti 3C2 nanoplatelets of the support matrix prepared in example 4. As can be seen from fig. 1, the Ti 3C2 material shows a layered structure under a high-power scanning electron microscope, and the thickness of the layered structure two-dimensional nano-sheet is less than 50: 50 nm.
Figure 2 XRD spectrum of layered Ti 3C2 nanoplatelets prepared in example 4. As can be seen from fig. 2, the Ti 3C2 material shows a Ti 3C2 spectral peak in the X-ray diffraction pattern.
Figure 3 is an XRD spectrum of final product D. As can be seen from fig. 3, the composite photocatalyst shows spectral peaks of BiVO 4, biOCl and Ti 3C2 in an X-ray diffraction pattern.
Fig. 4 is an SEM photograph of the final product D. As can be seen from fig. 4, the composite photocatalyst shows a laminated structure under a high-power scanning electron microscope, in which the surface of the support matrix Ti 3C2 is uniformly covered with a mesoporous film.
Fig. 5 is a TEM photograph of the final product D. As can be seen from fig. 5, the composite photocatalyst showed that the Ti 3C2 surface mesoporous film consisted of BiVO 4 and BiOCl particles less than 10 nm under high-power transmission electron microscopy.
Fig. 6 is a pore size distribution curve of the final product D. As can be seen from fig. 6, the pore size distribution range of the composite photocatalyst is 2.5-20 nm, and the composite photocatalyst has a mesoporous structure.
The mesoporous film laminated composite photocatalyst prepared in examples 1-4 is used for photocatalytic decomposition of water to produce hydrogen, and the reaction conditions are as follows:
the mesoporous film laminated composite photocatalyst prepared in the above examples 1-4 is respectively put into a quartz bottle, 300 mL distilled water is added, 4g sodium sulfide and 2 g sodium sulfite are added and dissolved in the distilled water to be used as a photocatalysis sacrificial agent, a 500W xenon lamp is used for experiment to simulate sunlight, the light intensity is 100 mW ∙ cm -2, nitrogen is firstly introduced for purging 30min before the reaction, then the photocatalysis continuous reaction is started for 48 h, the generated gas is collected, the volume is measured, and the gas composition is analyzed by gas chromatography. The hydrogen production amounts of the mesoporous film laminated composite photocatalysts prepared in examples 1 to 4 are shown in Table 1.
TABLE 1
| Examples | Sample of | Continuous reaction time (h) | Hydrogen production (mu mol) |
| Example 1 | Mesoporous film laminated composite photocatalyst A | 48 | 1091 |
| Example 2 | Mesoporous film laminated composite photocatalyst B | 48 | 1406 |
| Example 3 | Mesoporous film laminated composite photocatalyst C | 48 | 1756 |
| Example 4 | Mesoporous film laminated composite photocatalyst D | 48 | 1890 |
As shown in Table 1, when the mesoporous film laminated composite photocatalyst is used for decomposing water into hydrogen by photocatalysis, the photocatalytic efficiency is high, and the hydrogen production amount in 48 hours is more than 1000 mu mol by the catalysis of the photocatalyst, which is obviously superior to the photocatalyst in the prior art.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (3)
1. A laminated composite photocatalyst with mesoporous film, characterized in that: the composite photocatalyst consists of a carrier matrix, a surface coating and a binder, and has a laminated structure; the carrier matrix accounts for 68.0-99.0% of the weight of the composite photocatalyst, the surface coating accounts for 0.5-30.0% of the weight of the composite photocatalyst, and the binder accounts for 0.5-2.0% of the weight of the composite photocatalyst; the carrier matrix is a layered Ti 3C2 nanometer sheet, and the thickness of a single sheet layer in the layered structure of the layered Ti 3C2 nanometer sheet is 1-200 nm; the surface coating is a mesoporous film, and the aperture of the mesoporous film is 2-40 nm; the binder is perfluorinated sulfonic acid resin; the preparation method of the laminated composite photocatalyst with the mesoporous film comprises the following steps:
(1) Adding 40-60% hydrofluoric acid of 40-100 mL into a plastic beaker, weighing 5-10 g Ti 3AlC2, mixing with the hydrofluoric acid, stirring the mixed solution for uniform mixing for 20-60 min, transferring the uniformly mixed solution into a stainless steel reaction kettle for further reaction, centrifuging, treating at 80-160 ℃ by using a vacuum drying box, and finally cooling the material to obtain a carrier matrix layered Ti 3C2 nano sheet;
(2) Weighing 9-40 mg Bi (NO 3)3•5H2 O is dissolved in 10-60 mL concentration 1-4 mol/L dilute nitric acid, then 2-18 mg ammonium vanadate is added, room temperature magnetic stirring is carried out, 10-60 min is carried out, the pH value range of a solution system is regulated to 3-6 by using dilute hydrochloric acid, then 100 mg is weighed, the carrier substrate layered Ti 3C2 nano-sheets obtained in the step (1) are added with adhesive, then stirring is continued, after stirring, the liquid is transferred to a reaction kettle, 100-180 ℃ is reacted for 12-48 h, then the material is cooled at room temperature, distilled water and ethanol are respectively used for washing for two-three times, then the obtained product is placed in a vacuum drying box, the temperature is regulated to 60-120 ℃ and dried under vacuum condition for 8-24 h, finally, the obtained powder is transferred to a tubular furnace, and calcined for 6-12 h under the protection of argon gas, thus obtaining the laminated composite photocatalyst with a porous membrane.
2. The laminated composite photocatalyst with mesoporous film according to claim 1, wherein: the carrier matrix accounts for 84.0-94.5% of the weight of the composite photocatalyst, the surface coating accounts for 5.0-15.0% of the weight of the composite photocatalyst, and the binder accounts for 0.5-1.0% of the weight of the composite photocatalyst.
3. Use of the laminated composite photocatalyst with mesoporous membrane according to claim 1 for photocatalytic decomposition of aqueous hydrogen.
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