CN111408396A - Au/Cu5FeS4/g-C3N4Preparation method of plasma composite photocatalyst - Google Patents
Au/Cu5FeS4/g-C3N4Preparation method of plasma composite photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 46
- 229910052948 bornite Inorganic materials 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000002256 photodeposition Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000004729 solvothermal method Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000010931 gold Substances 0.000 abstract description 52
- 229910052737 gold Inorganic materials 0.000 abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000002784 hot electron Substances 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000004577 artificial photosynthesis Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
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- 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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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- 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
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Abstract
Au/Cu5FeS4/g‑C3N4The invention discloses a preparation method of a plasma composite photocatalyst, relates to a preparation method of a composite photocatalyst, and aims to provide a composite photocatalyst with g-C of a two-dimensional sheet structure3N4Based on the fact that the plasma gold nano-scale is uniformly attached to the g-C by adopting a photo-deposition method3N4On the sheet layer, and Cu is reacted by hydrothermal reaction5FeS4And coupling the nano particles to obtain the target photocatalyst. The method uses g-C3N4Au nanoparticles and Cu5FeS4Reacting under hydrothermal condition according to a certain molar ratio to form two-dimensional sheetg-C3N4 of the structure is taken as a basic support, and the plasma gold nanoparticles are uniformly attached to the g-C by adopting a photo-deposition method3N4On the sheet and with Cu5FeS4The nano particles are compounded, the prepared photocatalyst has a clear structure, and water can be decomposed by photocatalysis to generate hydrogen under the irradiation of visible light. The visible light photocatalyst has clear structure and definite composition.
Description
Technical Field
The invention relates to a preparation method of a composite photocatalyst, in particular to Au/Cu5FeS4/g-C3N4A preparation method of a plasma composite photocatalyst.
Background
The development and use of renewable energy are effective methods for solving the problem of environmental pollution due to the excessive use of fossil fuels. The hydrogen energy has the advantages of no pollution, recycling, wide raw material source, good combustion performance, high calorific value and the like, can release energy through direct combustion or in a hydrogen fuel cell, and the only product of hydrogen combustion is water which is an important raw material for preparing the hydrogen, so the hydrogen is a recyclable and sustainable energy source. The decomposition of water by solar energy to produce hydrogen, the so-called artificial photosynthesis, is undoubtedly one of the most important methods of solar energy conversion. In numerous studies, graphite phase carbon nitride (g-C)3N4) The photocatalyst has attracted much attention in photocatalysis due to the advantages of unique energy band structure and stable physicochemical properties. However, pure g-C3N4The photocatalytic performance is low, and two reasons mainly exist: (1) the light energy utilization rate is low. g-C3N4The forbidden band of (2.7 eV) is wide, and only light below 450 nm can be absorbed; (2) the light quantum efficiency is low. The photo-generated electron-hole pairs are very easy to recombine. Therefore, to increase g-C3N4The photocatalytic performance can be started from two aspects, and on one hand, the response range of the photocatalyst to visible light is widened; on the other hand, the separation efficiency of photon-generated carriers is improved, and the recombination of electron-hole pairs is inhibited. Under the irradiation of visible light, gold nanoparticles (Au NPs) can generate a local surface plasmon resonance effect due to electron resonance to excite "hot electrons". "Hot electrons" can be transferred from the Au NPs surface to g-C3N4The conduction band further participates in the photocatalytic reactionRealization of g-C3N4For larger wavelengths of visible light. Cu5FeS4Has relatively narrow band gap and excellent electronic conductivity, and introduces Cu into photocatalyst system5FeS4The transfer of photogenerated carriers can be effectively promoted, and the recombination of electron-hole pairs can be inhibited.
Disclosure of Invention
The invention aims to provide Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst takes g-C3N4Au nanoparticles and Cu5FeS4According to a certain mole ratio, reacting under hydrothermal condition to obtain g-C with two-dimensional sheet structure3N4For basic support, plasma gold nanoparticles (Au NPs) are uniformly attached to g-C by adopting a photo-deposition method3N4On the sheet and with Cu5FeS4The nano particles are compounded, the prepared photocatalyst has a clear structure, and water can be decomposed by photocatalysis to generate hydrogen under the irradiation of visible light.
The purpose of the invention is realized by the following technical scheme:
Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst comprises the following preparation steps:
(1) firstly, Cu is prepared by a solvothermal method5FeS4Nanoparticles; weighing CuCl and FeCl3·6H2O, respectively dispersing in ethylenediamine, ultrasonic treating, mixing the two solutions, and adding excessive (NH)4)2S solution; then transferring the solution into a reaction kettle with a polytetrafluoroethylene lining for reaction, washing black solids with deionized water and absolute ethyl alcohol in sequence, centrifuging, collecting precipitates, and drying overnight to obtain Cu5FeS4Nanoparticles; drying the obtained Cu5FeS4Adding water into the nano particles to prepare a solution;
(2) then weighing the g-C3N4Ultrasonically dispersed in L deionized water, and added thereto under stirring Au+Solution of Au/g-C by a photo-deposition method3N4The photocatalyst is sequentially washed by absolute ethyl alcohol and deionized water and dried;
(3) finally weighing the prepared Au/g-C3N4Adding water and performing ultrasonic treatment; under stirring, slowly adding Cu5FeS4Continuously stirring the solution, transferring the mixed solution to a reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction, naturally cooling to room temperature, sequentially washing the obtained product with deionized water and absolute ethyl alcohol, and drying to obtain Cu5FeS4Au/Cu as promoter5FeS4/g-C3N4A photocatalyst.
The Au/Cu5FeS4/g-C3N4Transferring the solution in the step (1) into a reaction kettle with a polytetrafluoroethylene lining, reacting for 24 hours at 180 ℃, and sequentially washing black solids for 3-5 times by using deionized water and absolute ethyl alcohol.
The Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst comprises the steps of (1) washing black solids with deionized water and absolute ethyl alcohol in sequence, centrifuging, collecting precipitates, and drying at 50 ℃ overnight to obtain Cu5FeS4Nanoparticles.
The Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst comprises the step (2) of Au/g-C3N4The photocatalyst is sequentially washed for 3-5 times by absolute ethyl alcohol and deionized water and is washed for 50 timesoAnd C, drying for 12 h.
The Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst comprises the step (3) of transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining for 180 DEG CoAnd C, performing hydrothermal reaction for 3 hours under the condition of C, and then naturally cooling to room temperature.
The Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst comprises the step of sequentially washing the product obtained in the step (3) with deionized water and absolute ethyl alcohol for 3-5 times, and washing the product at 50 DEGoDrying for 12 h under C to obtain Cu5FeS4Au/Cu as promoter5FeS4/g-C3N4A photocatalyst.
The invention has the advantages and effects that:
1. the invention adopts the Au NPs prepared by the photo-deposition method in the liquid, and the Au NPs stably exist in the solution and are not easy to agglomerate. Under the irradiation of visible light, the gold nanoparticles (Au NPs) can generate local surface plasma resonance effect due to electron resonance to excite 'hot electrons', so that g-C is realized3N4For larger wavelengths of visible light.
2. Due to Cu5FeS4The prepared Au/Cu has relatively narrow band gap and excellent electron conductivity, can effectively inhibit the recombination of electrons and holes, prolongs the service life, and thereby enhances the prepared Au/Cu5FeS4/g-C3N4The activity of the plasma composite photocatalyst under the catalysis of visible light.
3. The invention provides a new technical path for preparing the plasma composite photocatalyst and has important significance for solving the increasingly serious energy problem.
Drawings
FIG. 1 is Cu5FeS4/g-C3N4Transmission electron micrograph of Au photocatalyst.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, which, however, do not limit the scope of the invention.
g-C of the invention3N4Based Au/Cu5FeS4/g-C3N4And preparing the plasma composite photocatalyst, and applying the plasma composite photocatalyst to photocatalytic water decomposition for hydrogen production. g-C in a two-dimensional sheet-like structure3N4For basic support, plasma gold nanoparticles (Au NPs) are uniformly attached to g-C by adopting a photo-deposition method3N4On the sheet and with Cu5FeS4And (4) compounding the nano particles. The invention adopts a method of normal pressure and no additional assistance to prepare g-C with pure surface3N4A material. Then, a certain amount of AuCl is weighed3·HCl·4H2O and prepared g-C3N4The materials are evenly mixed in deionized water with the thickness of 20m L, ultrasonic treatment is carried out for 30min, after the materials are fully dispersed, the solution is transferred into a quartz reaction tank with the thickness of 100 m L, and Au/g-C is obtained by utilizing a photo-deposition method3N4A composite material. Meanwhile, Cu is prepared by a solvothermal method at 180 ℃ for 24 hours5FeS4Nanoparticles. Finally, a certain amount of newly prepared Cu is added5FeS4Dispersing the nanoparticles to Au/g-C3N4Mixing the materials uniformly, and adding the mixture to the mixture at 180 DEGoAnd C, carrying out hydrothermal reaction for 3 hours. Centrifuging the precipitate, sequentially cleaning with ethanol and deionized water, and drying to obtain Au/Cu5FeS4/g-C3N4A plasma composite photocatalyst.
Example 1
(1) Preparation of Cu by solvothermal method5FeS4Nanoparticles. First, 0.0990 g of CuCl and 0.2730 g of FeCl were weighed3·6H2O, respectively dispersing in ethylene diamine of 15 m L, mixing the two solutions after 15 min of ultrasonic treatment, and adding 4 times of excessive (NH)4)2And S, transferring the solution into a 50 m L polytetrafluoroethylene-lined reaction kettle, reacting at 180 ℃ for 24 hours, sequentially washing black solids for 3-5 times by using deionized water and absolute ethyl alcohol, centrifuging, collecting precipitates, and drying at 50 ℃ overnight to obtain Cu5FeS4Nanoparticles. Drying the obtained Cu5FeS430mg of the nano particles are weighed and added into 30ml of water to prepare a solution.
(2) Weighing 200 mg of g-C3N4Ultrasonically dispersed in 30m L deionized water, and 105 μ L Au was added thereto under stirring+(0.02428 mg/m L) by photo-deposition to give 0.25 wt% Au/g-C3N4Photocatalyst is prepared by mixing anhydrous alcohol and deionized waterWashing for 3-5 times at 50 deg.CoAnd C, drying for 12 h.
(3) 100 mg of the above-prepared 0.25 wt% Au/g-C was weighed3N420m L water was added and sonicated for 20min under stirring 0.75 m L Cu was added slowly5FeS4Stirring the solution for 30min, transferring the mixed solution into a 100 m L reaction kettle with polytetrafluoroethylene lining at 180%oPerforming hydrothermal reaction for 3 hours under the condition C, naturally cooling to room temperature, sequentially washing the obtained product for 3-5 times by using deionized water and absolute ethyl alcohol, and performing reaction at 50 DEGoDrying for 12 h at C to obtain Cu of 0.25 wt%5FeS40.25 wt% Au/0.75 wt% Cu of the cocatalyst5FeS4/g-C3N4A photocatalyst.
Example 2
As described in example 1, except that Au was added in the step (2)+Adjusted to 157. mu. L, the final catalyst was 0.5 wt% Au/0.75 wt% Cu containing 0.5 wt% Au5FeS4/g-C3N4A plasma composite photocatalyst.
Example 3
As described in example 1, except that Au was added in the step (2)+Adjusted to 209. mu. L, the final catalyst was 0.75 wt.% Au/0.75 wt.% Cu containing 0.75 wt.% Au5FeS4/g-C3N4A plasma composite photocatalyst.
Example 4
As described in example 1, except that Au was added in the step (2)+Adjusted to 418. mu. L, the final catalyst was 1 wt.% Au/0.75 wt.% Cu containing 1 wt.% Au5FeS4/g-C3N4A plasma composite photocatalyst.
Example 5
As described in example 1, except that Au was added in the step (2)+When the amount of (B) is adjusted to 627. mu. L, the final catalyst is 2 wt.% Au/0.75 wt.% Cu containing 2 wt.% Au5FeS4/g-C3N4A plasma composite photocatalyst.
Claims (6)
1. Au/Cu5FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized by comprising the following preparation steps:
(1) firstly, Cu is prepared by a solvothermal method5FeS4Nanoparticles; weighing CuCl and FeCl3·6H2O, respectively dispersing in ethylenediamine, ultrasonic treating, mixing the two solutions, and adding excessive (NH)4)2S solution; then transferring the solution into a reaction kettle with a polytetrafluoroethylene lining for reaction, washing black solids with deionized water and absolute ethyl alcohol in sequence, centrifuging, collecting precipitates, and drying overnight to obtain Cu5FeS4Nanoparticles; drying the obtained Cu5FeS4Adding water into the nano particles to prepare a solution;
(2) then weighing the g-C3N4Ultrasonically dispersed in L deionized water, and Au was added thereto under stirring+Solution of Au/g-C by a photo-deposition method3N4The photocatalyst is sequentially washed by absolute ethyl alcohol and deionized water and dried;
(3) finally weighing the prepared Au/g-C3N4Adding water and performing ultrasonic treatment; under stirring, slowly adding Cu5FeS4Continuously stirring the solution, transferring the mixed solution to a reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction, naturally cooling to room temperature, sequentially washing the obtained product with deionized water and absolute ethyl alcohol, and drying to obtain Cu5FeS4Au/Cu as promoter5FeS4/g-C3N4A photocatalyst.
2. Au/Cu according to claim 15FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized in that the solution in the step (1) is transferred into a reaction kettle with a polytetrafluoroethylene lining, and after the solution reacts for 24 hours at 180 ℃, black solid is usedAnd washing the mixture for 3-5 times by using deionized water and absolute ethyl alcohol in sequence.
3. Au/Cu according to claim 15FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized in that the black solid in the step (1) is sequentially washed by deionized water and absolute ethyl alcohol, centrifuged, collected and deposited, and dried at 50 ℃ overnight to obtain Cu5FeS4Nanoparticles.
4. Au/Cu according to claim 15FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized in that Au/g-C in the step (2)3N4The photocatalyst is sequentially washed for 3-5 times by absolute ethyl alcohol and deionized water and is washed for 50 timesoAnd C, drying for 12 h.
5. Au/Cu according to claim 15FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized in that the mixed solution in the step (3) is transferred into a reaction kettle with a polytetrafluoroethylene lining for 180 DEG CoAnd C, performing hydrothermal reaction for 3 hours under the condition of C, and then naturally cooling to room temperature.
6. Au/Cu according to claim 15FeS4/g-C3N4The preparation method of the plasma composite photocatalyst is characterized in that the product obtained in the step (3) is sequentially washed for 3-5 times by using deionized water and absolute ethyl alcohol and is washed for 50 timesoDrying for 12 h under C to obtain Cu5FeS4Au/Cu as promoter5FeS4/g-C3N4A photocatalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113134368A (en) * | 2021-03-22 | 2021-07-20 | 沈阳化工大学 | CdS/Cu5FeS4Preparation and application of/RGO nano composite photocatalyst |
| CN113134367A (en) * | 2021-03-22 | 2021-07-20 | 沈阳化工大学 | CdS/Cu5FeS4Preparation method of heterojunction semiconductor photocatalyst |
| CN114669328A (en) * | 2021-03-31 | 2022-06-28 | 北京理工大学 | Composite material photocatalyst for nitrogen reduction, preparation and application thereof |
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| CN106824243A (en) * | 2017-01-25 | 2017-06-13 | 东南大学 | Z-type BiVO4‑Au/g‑C3N4The preparation of catalysis material and its photo catalytic reduction CO2Application |
| CN109201102A (en) * | 2018-09-28 | 2019-01-15 | 商丘师范学院 | A kind of Z-type hetero-junctions M-C3N4The preparation method of/CdS composite photo-catalyst |
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