CN104069873A - Visible-light-induced photocatalyst loaded with vanadium tetrasulfide and preparation method - Google Patents
Visible-light-induced photocatalyst loaded with vanadium tetrasulfide and preparation method Download PDFInfo
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- CN104069873A CN104069873A CN201410275920.4A CN201410275920A CN104069873A CN 104069873 A CN104069873 A CN 104069873A CN 201410275920 A CN201410275920 A CN 201410275920A CN 104069873 A CN104069873 A CN 104069873A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a visible-light-induced photocatalyst loaded with four vanadium tetrasulfide (VS4) active component and a preparation method and belongs to the technical field of photocatalytic techniques. Graphene, carbon nano tube and silver sulfide are used as template carriers to improve the photocatalytic activity. The photocatalyst takes VS4 as the active component and the carbon nano tube as a carrier, and is prepared through a solvothermal method. The result shows that the prepared composite photocatalyst has good response at the visible light area and can effectively carry out water photolysis reaction; the success of the preparation of the photocatalyst has a certain theoretical and practical significance on sewage photocatalytic decomposition and hydrogen preparation through water photodecomposition for solving energy crisis.
Description
Technical field
The present invention relates to photocatalysis field, more particularly, relating to a kind of active ingredient is four vanadic sulfide (VS
4) preparation and the application thereof of visible light catalyst, catalyst can be used for carrying out the photocatalysis field researchs such as light degradation organic matter, photochemical catalyzing and application.
Background technology
Find TiO from researcher in 1972
2water can be decomposed into hydrogen and oxygen completely under ultraviolet lighting since, cause numerous researchers' concern for the research of conductor photocatalysis water decomposition.Hydrogen energy source has calorific value high (≈ 143kJ/g), and it is convenient to store, clean environment firendly, numerous advantages such as nonhazardous.
Under illumination condition, semi-conducting material outer-shell electron is excited, and transits to conduction band from valence band, forms electron-hole pair, and water is reduced into hydrogen by electronics, and hole Jiang Shui is oxidized to oxygen.To produce hydrogen and oxygen simultaneously, valence band current potential than oxygen current potential slightly just, and conduction band current potential is slightly more negative than hydrogen potential, the compound and photodissociation water of optical excitation electron-hole pair is a pair of competitive reaction in addition, and the existence of this reaction has also had a strong impact on the quantum efficiency of light.
But maximum composition that distributes in solar spectrum concentrates on visible region, therefore designing the catalyst in visible region with high quantum production rate is the key that makes full use of solar energy, reduces photocatalysis hydrogen production cost.And the narrow semiconductor less stable in forbidden band, easily because photoetch lost efficacy, and the suitable catalyst of part energy gap can not be realized release hydrogen oxygen simultaneously, thereby only has extremely minority semiconductor energy to realize a step decomposition water.
Research shows, part has the semiconductor of high response to sunshine, produces hydrogen and produces oxygen although can not a step realize, and under specific condition (have electron acceptor or electronics to and body), can realize efficient hydrogen manufacturing (or oxygen); After this more proposed the thought that two kinds of semiconductor combinations are used, simulating plant body photosynthetic " Z-type " photocatalysis system can realize hydrogen manufacturing and oxygen simultaneously.Meanwhile, under the photocatalysis being derived by photocatalytic water splitting hydrogen manufacturing (oxygen) half-reaction process, purifying the research of reproducibility (oxidisability) waste water also makes great progress.
VS
4be a kind of emerging semi-conducting material, there is very large specific area.Its energy gap is about 1.0eV, and visible ray is had to extremely strong response, can carry out under specific circumstances photocatalytic redox reaction.Need to about 1.8eV, in addition VS but water will be decomposed completely
4have stronger reproducibility, the hole forming in light-catalyzed reaction may be by its oxidation and therefore inactivation will be applied to photochemical catalyzing, needs further modification.
Summary of the invention
Technical problem: for improving visual efficiency, the present invention proposes a kind of visible light catalyst and preparation method who is loaded with four vanadic sulfides, described catalyst is using CNT, Graphene or silver sulfide particle as masterplate carrier, VS
4be monoclinic form in-situ crystallization in masterplate agent surface, catalyst has shown good activity in visible region, have higher quantum efficiency.
Technical scheme: in a kind of visible light catalyst that is loaded with four vanadic sulfides of the present invention, four vanadic sulfide VS
4nano particle exists with monocline crystalline phase, with Graphene rGO, CNT CNTs or silver sulfide Ag
2s particle, as masterplate carrier, forms VS
4/ rGO, VS
4/ CNTs, VS
4/ Ag
2s visible light catalyst, described VS
4/ rGO, VS
4/ CNTs, VS
4/ Ag
2rGO, CNTs and Ag in S
2the mass fraction of S masterplate carrier is 1.0%～10.0%.
The preparation method of a kind of visible light catalyst that is loaded with four vanadic sulfides of the present invention is: this catalyst is by solvent-thermal method one-step synthesis, and taking sodium orthovanadate as vanadium source, thioacetamide is sulphur source, and its raw material is calculated by weight and consisted of:
Sodium orthovanadate and thioacetamide are dissolved in to deionized water; The masterplate agent carrier adding, fully stirs 0.5～1.5h; Transfer in high temperature hydrothermal reaction kettle, 140～180 DEG C of insulation 12～48h, naturally cool to room temperature; Products therefrom is centrifugal, and with deionized water, ethanol washing, vacuum drying, grinds to obtain catalyst.
Visible light catalyst of the present invention is for visible light photocatalytic degradation industrial wastewater, agricultural effluent and photolysis water hydrogen solid/liquid/gas reactions.
Beneficial effect: Graphene is as template, and four vanadic sulfide particles are in its surface in situ crystallization; The introducing of Graphene can effectively promote separating of optical excitation electronics and hole, improves the quantum efficiency of catalyst.
Brief description of the drawings
Fig. 1 is rGO, VS
4/ rGO catalyst XRD figure.
Detailed description of the invention
Embodiment 1: visible light photocatalytic degradation formaldehyde-containing wastewater
Kaolinite Preparation of Catalyst as follows:
1) take 0.1343g CNT (CNTs), be scattered in 90mL deionized water, ultrasonic 0.5h forms uniform solution, stand-by;
2) take 2.7g 12 hydration sodium orthovanadates and 7.5g thioacetamide (CH
3cSNH
2), be dissolved in 1) gained solution, continue to stir 0.5h; Transfer in 150mL high temperature hydrothermal reaction kettle, 150 DEG C of insulation 12h, naturally cool to room temperature,
3) products therefrom is centrifugal, after washing, ethanol washing 3～5 times, 60 DEG C of vacuum drying 6h, grind containing the VS of 5% CNT
4catalyst.
Preparation is simulated industrial wastewater containing 1% formalin 500mL, adds the above-mentioned catalyst of 0.5g, with 500W high pressure xenon lamp (the following wavelength of elimination 400nm) simulated solar irradiation, carries out light-catalyzed reaction in 500mL photo catalysis reactor.
Every 1h sample analysis, draw contained formaldehyde mass fraction in solution by titration, and then calculate Degradation Formaldehyde rate.
After result shows 24h, Degradation Formaldehyde rate reaches 95.7%.
Embodiment 2: visible light catalytic decomposition water hydrogen producing
Kaolinite Preparation of Catalyst as follows:
1) take 0.0537g graphene oxide (GO), be scattered in 60mL deionized water, ultrasonic 1h forms uniform solution, stand-by;
2) take 1.8g Na
3vO
412H
2o and 1.65g CH
3cSNH
2, be dissolved in 1) and gained solution, continue to stir 1h; Transfer in 100mL high temperature hydrothermal reaction kettle, 160 DEG C of insulation 24h, naturally cool to room temperature,
3) products therefrom is centrifugal, after washing, ethanol washing 3～5 times, 60 DEG C of vacuum drying 6h, grind containing the VS of 3% Graphene
4catalyst.
Configuration is containing NaS
2concentration 0.35mol/L, Na
2sO
30.25mol/L solution 500mL, adds 0.5g catalyst, and the ultrasonic 0.5h of lucifuge, with 500W high pressure xenon lamp (the following wavelength of elimination 400nm) simulated solar irradiation, carries out light-catalyzed reaction, by gained gas collection, and uses gas chromatographic detection.Hydrogen maximum output reaches 600 μ mol/h.
Embodiment 3: visible light catalytic decomposing biomass ethanol hydrogen production
Kaolinite Preparation of Catalyst as follows:
1) take the ground silver sulfide powder of 0.0537g, be scattered in 60mL deionized water, ultrasonic 0.5h forms uniform solution, stand-by;
2) take 1.8g Na
3vO
412H
2o and 1.65g CH
3cSNH
2, be dissolved in 1) and gained solution, continue to stir 1.5h; Transfer in 100mL high temperature hydrothermal reaction kettle, 160 DEG C of insulation 48h, naturally cool to room temperature,
3) products therefrom is centrifugal, washing, ethanol wash after 3～5 times, and 60 DEG C of vacuum drying 6h grind containing 3%Ag
2the VS of S
4photochemical catalyst.
In 500mL photo catalysis reactor, add 0.5g catalyst, 500mL living beings ethanol, adds 0.1mol Na
2s fully mixes, and the ultrasonic 0.5h of lucifuge, with 500W high pressure xenon lamp (the following wavelength of elimination 400nm) simulated solar irradiation, carries out light-catalyzed reaction, will react gained and collect, and use gas chromatographic detection.Hydrogen maximum output reaches 350 μ mol/h.
Claims (3)
1. a visible light catalyst that is loaded with four vanadic sulfides, is characterized in that: in this catalyst, and four vanadic sulfide VS
4particle exists with monoclinic form, with reduced graphene rGO, CNT CNTs or silver sulfide Ag
2s particle, as masterplate carrier, forms VS
4/ rGO, VS
4/ CNTs, VS
4/ Ag
2s visible light catalyst, described VS
4/ rGO, VS
4/ CNTs, VS
4/ Ag
2rGO, CNTs and Ag in S
2the mass fraction of S masterplate carrier is 1.0%～10.0%.
2. the preparation method of an a kind of visible light catalyst that is loaded with four vanadic sulfides as claimed in claim 1, it is characterized in that: this catalyst is by solvent-thermal method one-step synthesis, taking sodium orthovanadate as vanadium source, thioacetamide is sulphur source, and its raw material is calculated by weight and consisted of:
Sodium orthovanadate and thioacetamide are dissolved in to deionized water; The masterplate agent carrier adding, fully stirs 0.5～1.5h; Transfer in high temperature hydrothermal reaction kettle, 140～180o is incubated 12～48h, naturally cools to room temperature; Products therefrom is centrifugal, and with deionized water, ethanol washing, vacuum drying, grinds to obtain catalyst.
3. an a kind of visible light catalyst that is loaded with four vanadic sulfides as claimed in claim 1 is for visible light photocatalytic degradation industrial wastewater, agricultural effluent and photolysis water hydrogen solid/liquid/gas reactions.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105618779A (en) * | 2014-11-07 | 2016-06-01 | 南京理工大学 | Preparation method of silver/reduced grapheme nanocomposite |
| CN105810942A (en) * | 2016-04-29 | 2016-07-27 | 陕西科技大学 | Preparation method of vanadium tetrasulfide nano-powder and application |
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| WO2017079868A1 (en) * | 2015-11-09 | 2017-05-18 | Robert Bosch Gmbh | Novel cathode and lithium ion rechargeable cells |
| CN107010666A (en) * | 2017-05-24 | 2017-08-04 | 岭南师范学院 | A kind of stalactite vanadic sulfide nano material and its preparation method and application |
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
| CN108352510A (en) * | 2015-11-09 | 2018-07-31 | 罗伯特·博世有限公司 | All solid state rechargeable lithium battery |
| WO2018181698A1 (en) * | 2017-03-31 | 2018-10-04 | 国立研究開発法人産業技術総合研究所 | Low crystallinity vanadium sulfide |
| CN108889310A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalysis composite film and preparation method thereof |
| CN108889311A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band optic catalytic composite material and preparation method thereof |
| CN108889312A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalytic nanometer array and preparation method thereof |
| CN109012697A (en) * | 2018-08-04 | 2018-12-18 | 徐靖才 | A kind of sunlight all band TiO2/VS4The preparation method of photochemical catalyst |
| CN109148857A (en) * | 2018-08-28 | 2019-01-04 | 中南大学 | A kind of preparation method of four vanadic sulfides of anode material of lithium-ion battery/carbon nanotube |
| CN109748319A (en) * | 2019-02-26 | 2019-05-14 | 陕西科技大学 | A kind of preparation method and application of four vanadic sulfides@carbon nano-tube composite powder |
| CN109999838A (en) * | 2019-05-09 | 2019-07-12 | 江苏纳欧新材料有限公司 | A kind of wide spectrum response vanadic sulfide/palygorskite nano composite material preparation method and application |
| CN110180556A (en) * | 2019-05-28 | 2019-08-30 | 广州大学 | A kind of four vanadic sulfide fenton catalyst of modification and its preparation method and application |
| CN112678870A (en) * | 2020-12-28 | 2021-04-20 | 北京理工大学 | Aluminum secondary battery and aluminum storage active material thereof |
| CN113413906A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
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Cited By (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105618779A (en) * | 2014-11-07 | 2016-06-01 | 南京理工大学 | Preparation method of silver/reduced grapheme nanocomposite |
| CN108352510A (en) * | 2015-11-09 | 2018-07-31 | 罗伯特·博世有限公司 | All solid state rechargeable lithium battery |
| WO2017079868A1 (en) * | 2015-11-09 | 2017-05-18 | Robert Bosch Gmbh | Novel cathode and lithium ion rechargeable cells |
| CN108352510B (en) * | 2015-11-09 | 2021-06-15 | 罗伯特·博世有限公司 | All-solid-state rechargeable lithium battery |
| CN105810942A (en) * | 2016-04-29 | 2016-07-27 | 陕西科技大学 | Preparation method of vanadium tetrasulfide nano-powder and application |
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| CN105923652B (en) * | 2016-04-29 | 2018-02-09 | 陕西科技大学 | A kind of multilevel hierarchy VS4Nano-powder and its preparation method and application |
| JPWO2018181698A1 (en) * | 2017-03-31 | 2020-02-13 | 国立研究開発法人産業技術総合研究所 | Low crystalline vanadium sulfide |
| WO2018181698A1 (en) * | 2017-03-31 | 2018-10-04 | 国立研究開発法人産業技術総合研究所 | Low crystallinity vanadium sulfide |
| CN107010666B (en) * | 2017-05-24 | 2019-05-21 | 岭南师范学院 | A kind of stalactite vanadic sulfide nano material and its preparation method and application |
| CN107010666A (en) * | 2017-05-24 | 2017-08-04 | 岭南师范学院 | A kind of stalactite vanadic sulfide nano material and its preparation method and application |
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
| CN109012697B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Sunlight all-band TiO2/VS4Method for preparing photocatalyst |
| CN108889312B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Preparation method of sunlight full-waveband photocatalytic nano array |
| CN108889310A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalysis composite film and preparation method thereof |
| CN109012697A (en) * | 2018-08-04 | 2018-12-18 | 徐靖才 | A kind of sunlight all band TiO2/VS4The preparation method of photochemical catalyst |
| CN108889311B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Preparation method of sunlight full-waveband photocatalytic composite material |
| CN108889311A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band optic catalytic composite material and preparation method thereof |
| CN108889312A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalytic nanometer array and preparation method thereof |
| CN108889310B (en) * | 2018-08-04 | 2020-11-10 | 中国计量大学 | Preparation method of sunlight full-waveband photocatalytic composite film |
| CN109148857A (en) * | 2018-08-28 | 2019-01-04 | 中南大学 | A kind of preparation method of four vanadic sulfides of anode material of lithium-ion battery/carbon nanotube |
| CN109748319A (en) * | 2019-02-26 | 2019-05-14 | 陕西科技大学 | A kind of preparation method and application of four vanadic sulfides@carbon nano-tube composite powder |
| CN109999838A (en) * | 2019-05-09 | 2019-07-12 | 江苏纳欧新材料有限公司 | A kind of wide spectrum response vanadic sulfide/palygorskite nano composite material preparation method and application |
| CN110180556A (en) * | 2019-05-28 | 2019-08-30 | 广州大学 | A kind of four vanadic sulfide fenton catalyst of modification and its preparation method and application |
| CN110180556B (en) * | 2019-05-28 | 2022-03-11 | 广州大学 | Modified vanadium tetrasulfide Fenton catalyst and preparation method and application thereof |
| CN112678870A (en) * | 2020-12-28 | 2021-04-20 | 北京理工大学 | Aluminum secondary battery and aluminum storage active material thereof |
| CN113413906A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
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Application publication date: 20141001 |