CN111957349A - Preparation method and application of photocatalytic water decomposition nanocomposite - Google Patents
Preparation method and application of photocatalytic water decomposition nanocomposite Download PDFInfo
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- CN111957349A CN111957349A CN202010672148.5A CN202010672148A CN111957349A CN 111957349 A CN111957349 A CN 111957349A CN 202010672148 A CN202010672148 A CN 202010672148A CN 111957349 A CN111957349 A CN 111957349A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 25
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- UKCIUOYPDVLQFW-UHFFFAOYSA-K indium(3+);trichloride;tetrahydrate Chemical compound O.O.O.O.Cl[In](Cl)Cl UKCIUOYPDVLQFW-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000012467 final product Substances 0.000 claims abstract description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000004070 electrodeposition Methods 0.000 claims description 3
- 238000003746 solid phase reaction Methods 0.000 claims description 3
- 238000012719 thermal polymerization Methods 0.000 claims description 3
- 238000004729 solvothermal method Methods 0.000 claims description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims 1
- 229910021617 Indium monochloride Inorganic materials 0.000 abstract description 6
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000000527 sonication Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 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
- 239000002131 composite material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/226—Sulfur, e.g. thiocarbamates
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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
- B01J27/24—Nitrogen compounds
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/30—Complexes comprising metals of Group III (IIIA or IIIB) as the central metal
- B01J2531/33—Indium
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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
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- 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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Abstract
The invention discloses a preparation method and application of a nano composite material for photocatalytic water decomposition, wherein the preparation method comprises the following steps: indium trichloride tetrahydrate (InCl)34H2O) ultrasonically dissolving the mixture in an ethylene glycol solution to set the mixture as a solution A; g to C3N4Dispersing in glycol solution, adding AgNO3Set as solution B; slowly pouring the solution B into the solution A, adding thioacetamide, and reacting to obtain the final product. The invention has the advantages that: 1. the prepared material has regular shape; 2. the prepared material has high efficiency of photocatalytic water decomposition; 3. the prepared material can be used for photocatalytic full-decomposition of water to realize fractional production of H2And produce O2Avoid H2And O2Separating; 4. the material is simple to prepare, low in cost and suitable for large-area popularization and application.
Description
Technical Field
The invention belongs to the technical field of energy environmental protection, and particularly relates to a preparation method and application of a photocatalytic water decomposition nanocomposite.
Background
With the over consumption of global fossil energy and the consequent environmental pollution problem, the search for green and renewable clean energy becomes a research hotspot in the field of energy environmental protection. The water resource on earth is rich, and water is decomposed into H by photocatalysis2And O2The solar energy which is almost inexhaustible can be directly converted into chemical energy to be stored. When the stored chemical energy needs to be released for use, H can be released2And O2Combusted and the resulting product is clean H2And O, realizing the circulation of the substances. Therefore, the development of the photocatalytic full water decomposition technology has important significance for solving the problems of energy shortage and environmental pollution at present.
The photocatalytic total water decomposition process consists of two parts, namely a Hydrogen Evolution Reaction (HER) and an Oxygen Evolution Reaction (OER). Where the OER reaction is a four-electron reaction process, the kinetics are slow, making it often the rate-limiting step for the total decomposition of water. And H2O is photooxidized to H2O2The process of (a) is a two-electron reaction process, which is relatively more likely to occur. Generation of H2O2Under the catalysis of a plurality of cheap catalysts such as MnO2, O is easily released2. Thus, H can be catalyzed by light2O implementation of first generation H2Reproduction of O2. Generation of H2And O2Can not be mixed together, and avoids the trouble caused by separation. Thus, photocatalytic water is first decomposed to H2And H2O2Then catalyzes H2O2Produce O2To realize indirect photocatalysis H2Decomposition of O to H2And O2Becoming a research hotspot in the field today. The development of corresponding water decomposing materials with low cost and high efficiency and the improvement of the water decomposing efficiency by photocatalysis become important research contents in the field.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method and application of a photocatalytic water decomposition nano composite material, and a prepared photocatalytic water decomposition nano composite materialThe composite material can be used for producing H by steps through photocatalytic water decomposition2And O2And the catalytic efficiency is high.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a nano composite material for photocatalytic water decomposition is characterized by comprising the following preparation steps:
(1) preparation of g-C by methods of the prior art3N4For example, g-C is prepared by one of solid-phase reaction, solvothermal, electrochemical deposition, and thermal polymerization3N4。
(2) Adding proper amount of indium trichloride tetrahydrate (InCl)34H2O) ultrasonically dissolving in 25mL of glycol solution, setting the solution A as the solution, and adding 5-50 mmol of indium trichloride tetrahydrate;
(3) taking g-C prepared by the step (1)3N4Dispersing 10-100 mg of ultrasonic wave in 25mL of ethylene glycol solution, and adding 1-10 mmol of AgNO3Set as solution B;
(4) and slowly pouring the solution B into the solution A, stirring, adding 3-30 mmol of thioacetamide, carrying out magnetic stirring for 3 hours in a water bath at 70-90 ℃, aging, centrifuging, washing, filtering, and drying at 50-70 ℃ to obtain a final product.
The application of the photocatalytic water splitting nanocomposite prepared by the preparation method is characterized in that: the nano composite material for photocatalytic water decomposition can be used for high-efficiency photocatalytic water decomposition to produce H step by step2And O2. First generation H2Reproduction of O2Can avoid H2And O2And (5) separating.
The invention has the advantages that: 1. the prepared material has regular shape; 2. the prepared material has high efficiency of photocatalytic water decomposition; 3. the prepared material is particularly suitable for photocatalytic full water decomposition to realize fractional production of H2And produce O2Avoid H2And O2Separating; 4. the material is simple to prepare, low in cost and suitable for large-area popularization and application.
Drawings
FIG. 1 is a scanning electron micrograph of a product according to example 3 of the present invention;
FIG. 2 shows the photocatalytic decomposition of water H by the product of example 3 of the present invention2And O2The yield map of (a).
Detailed Description
The technical solution of the present invention will be described in detail with reference to the specific embodiments of the present application. However, the scope of the present invention is not limited to the following specific examples.
Example 1
Synthesis of g-C by solid phase reaction3N4。
5 mmol of indium trichloride tetrahydrate (InCl)3·4H2O) was dissolved in 25mL of an ethylene glycol solution with sonication to obtain solution A. Respectively taking 10mg of g-C3N4Dissolving in 25mL of glycol solution, performing ultrasonic dispersion, and collecting 1 mmol of AgNO3Adding the above solution, and performing ultrasonic treatment for 1min to dissolve, to obtain solution B. Slowly pouring the solution B into the solution A, stirring, adding 3 mmol of thioacetamide, performing magnetic stirring in a water bath at 70 ℃ for 3 hours, aging, centrifuging, washing, filtering, and drying at 50 ℃ to obtain a final product.
Example 2
Synthesis of g-C by solvothermal method3N4。
10 mmol of indium trichloride tetrahydrate (InCl)3·4H2O) was dissolved in 25mL of an ethylene glycol solution with sonication to obtain solution A. Respectively taking 20mg of g-C3N4Dissolving in 25mL of glycol solution, performing ultrasonic dispersion, and taking 2 mmol of AgNO3Adding the above solution, and performing ultrasonic treatment for 1min to dissolve, to obtain solution B. Slowly pouring the solution B into the solution A, stirring, adding 10 mmol of thioacetamide, performing magnetic stirring in a water bath at 90 ℃ for 3 hours, aging, centrifuging, washing, filtering, and drying at 70 ℃ to obtain a final product.
Example 3
Synthesis of g-C by electrochemical deposition3N4。
30 mmol of tetrahydrateIndium trichloride (InCl)3·4H2O) was dissolved in 25mL of an ethylene glycol solution with sonication to obtain solution A. Respectively taking 50mg of g-C3N4Dissolving in 25mL of glycol solution, performing ultrasonic dispersion, and taking 8 mmol of AgNO3Adding the above solution, and performing ultrasonic treatment for 1min to dissolve, to obtain solution B. Slowly pouring the solution B into the solution A, stirring, adding 20 mmol of thioacetamide, performing magnetic stirring in a water bath at 80 ℃ for 3 hours, aging, centrifuging, washing, filtering, and drying at 60 ℃ to obtain a final product.
Example 4
Synthesis of g-C by thermal polymerization3N4。
50 mmol of indium trichloride tetrahydrate (InCl)3·4H2O) was dissolved in 25mL of an ethylene glycol solution with sonication to obtain solution A. Respectively taking 100mg of g-C3N4Dissolving in 25mL of glycol solution, performing ultrasonic dispersion, and taking 10 mmol of AgNO3Adding the above solution, and performing ultrasonic treatment for 1min to dissolve, to obtain solution B. Slowly pouring the solution B into the solution A, stirring, adding 30 mmol of thioacetamide, performing magnetic stirring in a water bath at 80 ℃ for 3 hours, aging, centrifuging, washing, filtering, and drying at 60 ℃ to obtain a final product.
The prepared nano composite material for photocatalytic water decomposition can be used for high-efficiency photocatalytic water decomposition to produce H step by step2And O2. First generation H2Reproduction of O2Can avoid H2And O2And (5) separating.
FIG. 1 is a scanning electron microscope image of the product of example 3, from which it can be seen that the morphology of the material is uniform and regular.
FIG. 2 shows the photocatalytic decomposition of water H by the product of example 3 of the present invention2And O2The yield map of (a).
The foregoing is a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations are also regarded as the protection scope of the present invention.
Claims (3)
1. A preparation method of a nano composite material for photocatalytic water decomposition is characterized by comprising the following preparation steps:
(1) preparation of g-C by methods of the prior art3N4；
(2) Adding proper amount of indium trichloride tetrahydrate InCl34H2Dissolving O in 25mL of glycol solution by ultrasonic treatment, setting the solution A as the solution, and adding 5-50 mmol of indium trichloride tetrahydrate;
(3) taking g-C prepared by the step (1)3N4Dispersing 10-100 mg of ultrasonic wave in 25mL of ethylene glycol solution, and adding 1-10 mmol of AgNO3Set as solution B;
(4) and slowly pouring the solution B into the solution A, stirring, adding 3-30 mmol of thioacetamide, carrying out magnetic stirring for 3 hours in a water bath at 70-90 ℃, aging, centrifuging, washing, filtering, and drying at 50-70 ℃ to obtain a final product.
2. The method for preparing a nanocomposite material for photocatalytic water splitting according to claim 1, wherein: the prior art in the step (1) is any one of a solid-phase reaction method, a solvothermal method, an electrochemical deposition method and a thermal polymerization method.
3. The use of the photocatalytic water splitting nanocomposite material prepared by the preparation method according to claim 1, wherein: the nano composite material for photocatalytic water decomposition can be used for high-efficiency photocatalytic water decomposition to produce H step by step2And O2。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018020356A1 (en) * | 2016-07-28 | 2018-02-01 | Sabic Global Technologies B.V. | Nitrogen rich carbon nitride materials with a three dimensional cubic mesoporosity from diaminotetrazine |
| CN108993564A (en) * | 2018-07-02 | 2018-12-14 | 江苏大学 | In situ synthesis one-step synthesis quantum dot/nanometer sheet heterojunction composite photocatalyst |
| CN110227552A (en) * | 2019-07-10 | 2019-09-13 | 西北师范大学 | A kind of preparation method of BCN@AZIS composite catalyst |
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- 2020-07-14 CN CN202010672148.5A patent/CN111957349A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018020356A1 (en) * | 2016-07-28 | 2018-02-01 | Sabic Global Technologies B.V. | Nitrogen rich carbon nitride materials with a three dimensional cubic mesoporosity from diaminotetrazine |
| CN108993564A (en) * | 2018-07-02 | 2018-12-14 | 江苏大学 | In situ synthesis one-step synthesis quantum dot/nanometer sheet heterojunction composite photocatalyst |
| CN110227552A (en) * | 2019-07-10 | 2019-09-13 | 西北师范大学 | A kind of preparation method of BCN@AZIS composite catalyst |
Non-Patent Citations (2)
| Title |
|---|
| XIAOXUE LI ET AL.: "Enhanced Photocarrier Separation in Hierarchical Graphitic-C3N4-Supported CuInS2 for Noble-Metal-Free Z-Scheme Photocatalytic Water Splitting", 《ACS APPL. MATER. INTERFACES》 * |
| 张燕: "硫化铟银基光催化剂的制备及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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