CN111957334A - Preparation method of composite ternary heterojunction photocatalyst - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title claims abstract description 11
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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
-
- B01J35/39—
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
Abstract
A preparation method of a composite ternary heterojunction photocatalyst relates to a preparation method of a photocatalyst, and the invention uses Ag+The method comprises the following steps of reacting a zinc source, an indium source, a sulfur source, graphene and graphite-phase carbon nitride according to a certain proportion under a hydrothermal condition to obtain a target photocatalyst. Ternary heterojunction Ag: ZnIn2S4/RGO/g‑C3N4g-C of photocatalyst under irradiation of visible light3N4And Ag ZnIn2S4Both components are excited and produce photo-generated electrons and holes. Meanwhile, RGO can be used as a bridge in the case of Ag: ZnIn2S4And g-C3N4Realize obvious connection between the two, and is favorable for the conversion of current carriersAnd the photocatalytic hydrogen production performance is improved. Ternary heterojunction Ag: ZnIn2S4/RGO/g‑C3N4The photocatalyst has good capability of producing hydrogen by decomposing water through visible light photocatalysis, has wide prospect in the aspects of clean energy production and energy conversion, and is a future bright catalyst.
Description
Technical Field
The invention relates to a preparation method of a photocatalyst, in particular to a preparation method of a composite ternary heterojunction photocatalyst.
Background
Energy and environmental crisis are affecting human survival and development. Semiconductor photocatalytic technology is considered as one of the most effective means for solving the above problems. In order to improve the light conversion efficiency of solar energy, a large number of photocatalysts are explored and constructed. The traditional single photocatalyst has the defects of fast carrier recombination, narrow spectral response and the like. In recent years, a great deal of research has found that the diversity of composite photocatalytic systems and good charge separation efficiency are key strategies to solve the above problems.
Graphite phase nitrogen carbide (g-C)3N4) The photocatalyst is considered to be the most promising visible light photocatalyst due to the characteristics of unique electronic structure, high stability, no toxicity, low cost and the like. However, since a single component g-C3N4The specific surface area is small, the recombination rate of photo-generated electron-hole pairs is high, and the like, so that the photocatalytic hydrogen production efficiency is still not ideal so far, and the development of the photocatalytic hydrogen production efficiency in the field of photocatalytic hydrogen production is limited. Recent studies have found that3N4In the photocatalytic modification, designing and constructing a proper heterojunction is considered to be a low-cost and effective improvement of g-C3N4Method of photocatalyst activity. In general, g-C3N4The base heterojunction can not only inhibit the recombination of photoinduced carriers by forming a tight interface, but also can impart some unique properties to the photocatalyst. Thus, g-C3N4The reasonable construction of the base heterostructure provides a feasible approach for developing the high-efficiency visible light response photocatalyst.
Recently, the ternary sulfur compound (abbreviated as AB)2X4A = Zn, Ca, Cu, Cd; b = Al, Ga, in; x = S, Se, Te) has a layered structure of ZnIn2S4With its excellent electrical and optical properties, it is widely studied as an eco-friendly visible light drive photocatalyst. Thus, ZnIn2S4The base semiconductor material is widely applied to the aspect of photocatalytic hydrogen production. In addition, Ag+Having a 4d electronic structure in ZnIn2S4Middle doped with a small amount of Ag+Not only can generate Ag4d donor energy level, broadens the spectral response range and improves the utilization rate of photo-generated electrons. In addition, lattice defects may be generated on the surface of the semiconductor, thereby forming more oxidation centers, inhibiting recombination of electrons and holes, and improving photocatalytic activity.
Graphene (RGO) has the advantages of large specific surface area, high conductivity, good stability, adjustable surface properties, and the like, and is considered to be a novel cocatalyst. Researches find that graphene can be introduced into various semiconductor photocatalysts to form a graphene-based composite semiconductor photocatalyst, and due to the excellent carrier mobility, the diffusion range of photogenerated carriers can be enlarged, the recombination of electrons and holes is inhibited, the service life is prolonged, and the graphene has more excellent photocatalytic performance.
Disclosure of Invention
The invention aims to provide a preparation method of a composite ternary heterojunction photocatalyst, which utilizes a small amount of Ag to ZnIn2S4With RGO and g-C3N4A heterojunction is formed. The photocatalyst has obviously improved hydrogen production activity, and is applied to photocatalytic hydrogen production.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a composite ternary heterojunction photocatalyst comprises the following preparation processes:
firstly, Graphene Oxide (GO) is synthesized by adopting a modified Hummers method and g-C is synthesized by utilizing a thermal polymerization method3N4Nanosheets, then, mixing GO with g-C3N4Ultrasonically dispersing in distilled water; next, Zn (OAc) was added thereto2， In(OAc)3，AgNO3And L-cysteine, then adding thioacetamide, and transferring the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining; after the hydrothermal reaction, the precipitate is centrifugally separated, washed with deionized water for several times, and dried to obtain the ternary heterojunction Ag: ZnIn2S4/RGO/g-C3N4A photocatalyst.
The invention has the advantages and effects that:
(1) ag can be prepared by a hydrothermal method+Homogeneous and stable doping to ZnIn2S4In the method, an Ag4d donor level can be generated in the semiconductor, and photons with smaller energy can excite the energy level to generate electrons and holes under the irradiation of visible light, so that the utilization rate of the photons is improved, and the visible light catalytic reaction is promoted.
(2) The prepared ternary heterojunction Ag is ZnIn2S4/RGO/g-C3N4Photocatalyst having a ratio of Ag to ZnIn2S4/g-C3N4And RGO/g-C3N4The heterojunction photocatalyst has higher visible light catalytic hydrogen production performance, and Ag is ZnIn2S4/RGO/g-C3N4The photocatalytic activity of the novel heterojunction catalyst greatly exceeds that of a pure physical mixture thereof.
(3) Ternary heterojunction Ag: ZnIn2S4/RGO/g-C3N4g-C of photocatalyst under irradiation of visible light3N4And Ag ZnIn2S4Both components are excited and produce photogenerated electrons and holes, and RGO can be used as a bridge in the case of ZnIn2S4And g-C3N4The obvious connection is realized, which is beneficial to the transfer of current carriers, thereby improving the photocatalytic hydrogen evolution performance.
(4) The invention adopts a common hydrothermal synthesis method to synthesize Ag, ZnIn2S4/RGO/g-C3N4The heterojunction photocatalyst has high crystallinity, good dispersibility, controllable shape, common raw materials, controllable process and easy implementation, and meets the requirement of environmental friendliness.
The invention provides a new technical path for developing the visible light semiconductor photocatalysis field, and has important significance for solving the increasingly serious energy problem.
Drawings
FIG. 1 shows the Ag-ZnIn of the present invention2S4/RGO/g-C3N4Transmission electron micrograph of the heterojunction photocatalyst.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention relates to Ag ZnIn2S4Semiconductor with Reduced Graphene (RGO) and graphite phase nitrogen carbide (g-C)3N4) Preparation method of composite ternary heterojunction photocatalyst by using Ag+The zinc source, the indium source, the sulfur source, the graphene and the graphite-phase carbon nitride react in proportion under a hydrothermal condition, so that the target ternary heterojunction photocatalyst is obtained. The prepared ternary heterojunction photocatalyst has clear structure and composition, and can decompose water to generate hydrogen under the irradiation of visible light.
Example 1
(1) Preparing Graphene Oxide (GO). The graphene oxide is synthesized by taking nano graphite powder as a raw material and adopting a modified Hummers method. The GO brown powder is dispersed in water, and graphite oxide is exfoliated by ultrasonic action to prepare a monodisperse graphene oxide solution (1 g/L).
(2) Preparation of graphitic carbo-nitrides (g-C)3N4). We can obtain g-C by calcining a mass of urea3N4. In general, 5g of urea was placed in a foil-covered crucible, which was then placed in a muffle furnace at 2Heating at 50 deg.C for 1h, 350 deg.C for 2h, 550 deg.C for 2h, and heating at 1 deg.C for min in air atmosphere-1. The yellow product was collected and ground to a powder for further use.
(3) ZnIn as ternary heterojunction Ag is synthesized by conventional hydrothermal method2S4/RGO/g-C3N4A photocatalyst. First, 0.75mg of GO and 119.25 mg g-C3N4Dispersed ultrasonically in 20ml of distilled water. The suspension was then transferred into a 100ml teflon stainless steel autoclave, sealed and kept at 160 ℃ for 6 h. Next, 1416. mu.L of 0.05 mmol/mL zinc acetate solution, 1416. mu.L of 0.1 mmol/mL indium acetate solution, 521. mu.L of 0.8 mmol/L silver nitrate solution, 944. mu.L of 0.01 mmol/mL L-cysteine were added to the synthesized RGO/g-C under stirring3N4After 30 minutes 2832. mu.L of a 0.1 mmol/mL thioacetamide solution was added, followed by standing at 160 ℃ for 6 hours. The product was collected by centrifugation, washed several times with deionized water to remove possible residual impurities, and then dried at 50 ℃ to give the final catalyst as 0.5 wt% Ag: ZnIn containing 0.5 wt% RGO2S4/RGO/g-C3N4。
Example 2
As described in example 1, except that 1.125mg of GO and 118.875 mg of g-C were added in step (3)3N4Dispersed ultrasonically in 20ml of distilled water, the final catalyst was 0.75 wt% Ag-ZnIn containing 0.75 wt% RGO2S4/RGO/g-C3N4。
Example 3
As described in example 1, except that 1.5mg of GO and 118.5 mg g-C were added in step (3)3N4Dispersed in 20ml of distilled water by sonication, the final catalyst was 1 wt% Ag-ZnIn containing 1 wt% RGO2S4/RGO/g-C3N4。
Example 4
As described in example 1, except that 3mg of GO and 117 mg g-C were added in step (3)3N4Ultrasonic dispersion in 20ml of distilled water to obtain the final catalystThe agent is 2 wt% Ag containing 2 wt% RGO and ZnIn2S4/RGO/g-C3N4。
Example 5
As described in example 1, except that 4.5mg of GO and 115.5mg g-C were added in step (3)3N4Dispersed in 20ml of distilled water by sonication, the final catalyst was 3 wt% Ag-ZnIn containing 3 wt% RGO2S4/RGO/g-C3N4。
Claims (1)
1. The preparation method of the composite ternary heterojunction photocatalyst is characterized in that the preparation method of the composite ternary heterojunction photocatalyst by a hydrothermal method comprises the following preparation processes:
firstly, Graphene Oxide (GO) is synthesized by adopting a modified Hummers method and g-C is synthesized by utilizing a thermal polymerization method3N4Nanosheets, then, mixing GO with g-C3N4Ultrasonically dispersing in distilled water; next, Zn (OAc) was added thereto2， In(OAc)3，AgNO3And L-cysteine, then adding thioacetamide, and transferring the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining; after the hydrothermal reaction, the precipitate is centrifugally separated, washed with deionized water for several times, and dried to obtain the ternary heterojunction Ag: ZnIn2S4/RGO/g-C3N4A photocatalyst.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113134378A (en) * | 2021-03-30 | 2021-07-20 | 沈阳化工大学 | W18O49/g-C3N4Preparation method of/RGO semiconductor photocatalyst |
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| CN110124693A (en) * | 2019-05-28 | 2019-08-16 | 沈阳化工大学 | The composite metal ion doped deficiency semiconductor light-catalyst preparation method of graphene |
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| CN103611548A (en) * | 2013-11-28 | 2014-03-05 | 福州大学 | Reduced graphene oxide/ZnIn2S4 photocatalyst and preparation method and application thereof |
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Cited By (1)
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