CN109174149A - A kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material and preparation method thereof - Google Patents
A kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material and preparation method thereof Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 77
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 77
- 239000000463 material Substances 0.000 title claims abstract description 65
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 44
- 150000001875 compounds Chemical class 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000004044 response Effects 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000011218 binary composite Substances 0.000 claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 33
- 239000011941 photocatalyst Substances 0.000 claims description 19
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 19
- 229940043267 rhodamine b Drugs 0.000 claims description 19
- 238000006731 degradation reaction Methods 0.000 claims description 17
- 230000015556 catabolic process Effects 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000000178 monomer Substances 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000004873 anchoring Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005297 material degradation process Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000011206 ternary composite Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000012546 transfer Methods 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
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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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- B01J35/39—
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The present invention relates to environment functional material fields, and in particular to a kind of visible-light response type MoS2/GO/g‑C3N4Tri compound catalysis material and preparation method thereof.The tri compound catalysis material is by MoS2, GO and g-C3N4It is combined；The MoS2Uniform load is on GO in the form of nano particle, and in GO and g-C3N4π-πconjugation under formed tight structure tri compound catalysis material.Photocatalytic Degradation Property experiment shows MoS provided by the present invention2/GO/g‑C3N4Tri compound catalysis material is relative to MoS2Or g-C3N4Monomer and MoS2/ GO binary composite catalyst all has the performance of more preferably photocatalytic degradation RhB, solar energy conversion and in terms of have a good application prospect and economic benefit.
Description
Technical field
The present invention relates to environment functional material fields, and in particular to a kind of visible-light response type MoS2/GO/g-C3N4Ternary
Composite photocatalyst material and preparation method thereof.
Background technique
With the fast development of global industry technology, problem of environmental pollution is increasingly serious, makes to people's health and life
At immeasurable harm.Therefore, pollution administration, protection environment have become one of the problem of people pay close attention to the most.It is several recently
Year, photocatalysis technology is grown rapidly, and becomes a kind of green technology for having important application prospect in the energy and environmental area.Wherein
Semiconductor light-catalyst the advantages that easy, energy consumption is less with its preparation, degradation speed is fast, is in the depollution of environment, field of solar energy conversion
It receives much attention.
Carbonitride (g-C3N4) it is used as a kind of novel metalloid catalyst, there is the layer structure of similar graphite, has excellent
Electrons transmittability, higher both thermally and chemically stability and narrow forbidden bandwidth (2.7-2.8eV), quilt
It is considered as a kind of potential visible-light-responsive photocatalyst.But at the same time, g-C3N4Quantum efficiency is low and light induced electron-
The recombination rate in hole pair is still higher.Some researches show that by g-C3N4Compound with other materials is to solve the problems, such as that this one kind is effective
Approach.In recent years, design utilizes molybdenum sulfide (MoS inexpensive, with excellent visible light absorption capacity2) it is used as co-catalysis
Agent causes the great interest of people to substitute noble metal as photochemical catalyst.
A kind of novel MoS is disclosed in the prior art2/g-C3N4Compound photochemical catalyst, the two is compound can to enhance boundary
Surface charge transfer rate and delay electron-hole pair (e--h+) recombination rate.Be also disclosed using combine hard mold plate technique and
The hollow MoS of one kind that the technology of dipping sulphur oxidizing process is successfully prepared2/g-C3N4Tri compound catalysis material, the catalyst by
In in MoS2And g-C3N4Between the film that is formed there is efficient carrier separation ability and more active sites, enhance
Visible light photocatalysis hydrogen manufacturing performance.
However MoS2And g-C3N4Between separation of charge and electron transfer rate and not up to our desired value.Aoxidize stone
Black alkene (GO) has received widespread attention because it has property similar with graphene, and a large amount of hydroxyl is introduced on the surface GO
Base and carboxylic group are more advantageous to anchoring nano material, improve the dispersibility and utilization rate of nano material.GO has stronger simultaneously
Light absorpting ability, be conducive to enhance the absorbability to visible light.Therefore, the present invention is by MoS2And g-C3N4Diploid
A kind of preferable GO of electric conductivity is added in system, further enhances material to the absorbability and photo-generate electron-hole of visible light
Pair separating capacity, improve photocatalytic degradation environmental contaminants ability.
Summary of the invention
It is an object of the invention to overcome technological deficiency existing in the prior art, MoS is solved2、g-C3N4Equal monomers photoproduction
Electron-hole low separation efficiency and MoS2/g-C3N4The not high problem of binary system catalytic efficiency.Improve the suction to visible light
Receipts ability and photoproduction electricity book-hole pair separative efficiency, to improve the performance of tri compound catalysis material and its steady
It is qualitative.
Above-mentioned technical purpose that the invention is realized by the following technical scheme:
On the one hand, the present invention provides a kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material, described three
First composite photocatalyst material is by MoS2/ GO binary composite and g-C3N4It is combined, wherein GO accounts for MoS2/ GO gross mass
1~7%；MoS2/ GO accounts for MoS2/GO/g-C3N4The 1 ~ 5% of tri compound catalysis material gross mass.
Preferably, the MoS2/GO/g-C3N4GO accounts for MoS in tri compound catalysis material2The 5% of/GO gross mass；
MoS2/ GO accounts for MoS2/GO/g-C3N4The 3 ~ 5% of Three-element composite photocatalyst gross mass.
On the other hand, the present invention provides a kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material
Preparation method, the preparation method comprises the following steps:
(1) by molybdenum trioxide (MoO3) be added in deionized water with potassium rhodanate (KSCN) and stir, mixed after ultrasonic disperse
Solution disperses GO in after ethylene glycol solution and is added in above-mentioned mixed solution, is fitted into kettle after continuation ultrasonic disperse and passes through solvent
MoS is prepared in thermal method2/ GO binary composite photocatalyst material；
(2) respectively by MoS obtained in above-mentioned steps (1)2/ GO binary composite photocatalyst material, g-C3N4It is added in ethylene glycol
Solution is fitted into reaction kettle after even stirring, ultrasonic disperse, MoS is prepared by solvent-thermal method2/GO/g-C3N4Tri compound
Catalysis material.
MoO described in above-mentioned steps (1)3Molar ratio with KSCN is 1:2.5；
GO and MoO described in above-mentioned steps (1)3Mass ratio be 1 ~ 7:144；
The proportionate relationship of GO and ethylene glycol is 0.001 ~ 0.007g:10mL in above-mentioned steps (1)；
MoS described in above-mentioned steps (2)2/ GO and g-C3N4Mass ratio be 1:99 ~ 5:95；
MoS described in above-mentioned steps (2)2The proportionate relationship of/GO and ethylene glycol is than 0.001 ~ 0.005g:20mL；
The reaction of baking oven described in above-mentioned steps (1), step (2) is to react for 24 hours at 180 DEG C of temperature.
In another aspect, the present invention also provides above-mentioned 3 ~ 5wt %MoS2/GO/g-C3N4The use of tri compound catalysis material
On the way, it is used for rhodamine B degradation (RhB), after radiation of visible light 5h, to the degradation rate for the rhodamine B (RhB) that concentration is 10mg/L
Reach 91.0 ~ 96.7%.
Compared with prior art, the medicine have the advantages that
(1) MoS2It can be improved the absorbability to visible light with relatively narrow forbidden bandwidth, with g-C3N4It is compound using respective
Advantage and the two synergistic effect enhancing photo-generate electron-hole pair separating capacity, improve photocatalysis performance；GO has big
Surface area and high electron mobility can not only provide load site for nano material as nonmetallic co-catalyst
The dispersibility and homogeneity for enhancing nano material, provide more active sites for the absorption and degradation of target contaminant, simultaneously
The transmission rate that electronics can be further enhanced improves quantum yield and visible light catalytic performance.
(2) MoS provided by the present invention2/GO/g-C3N4MoS in tri compound catalysis material2With the shape of nano particle
Formula uniform load is on GO, compared to monomer MoS2And binary system MoS2MoS in/GO2, MoS in ternary system2Ruler
Very little smaller and dispersion is more uniform, while GO and carrier material g-C3N4Under the action of π-is pi-conjugated combine it is even closer, it is this
Ternary structural system can effectively increase active site, but also the transmission rate of electronics is higher.It is multiple that ternary can finally be effectively improved
Condensation material enhances tri compound catalysis material to the absorbability of visible light and the separative efficiency of photo-generate electron-hole pair
Performance and its stability.
(3) MoS in the present invention2, GO and g-C3N4Simple and easy to get, the introducing of GO is conducive to MoS2Anchoring growth, make
MoS2Do not reunite and be intended to it is evenly dispersed and with small form of nanoparticles homoepitaxial on GO；It will in conjunction with solvent-thermal method
MoS2/ GO is supported on g-C3N4Surface；Due to MoS2And g-C3N4Position of energy band matching, and GO can be promoted material conduction son
Ability is finally reached the purpose for promoting photocatalysis performance.Photocatalytic Performance Study the result shows that, after radiation of visible light 5h,
The tri compound catalysis material reaches 96.7% to the degradation efficiency for the RhB solution that concentration is 10mg/L；Present invention preparation simultaneously
Ternary complex catalyst preparation method is easy to operate, reagent is cheap, can be used for large-scale low-cost preparation, turn in solar energy
Change and sewage treatment etc. have a good application prospect and economic benefit.
Detailed description of the invention
Fig. 1 is MoS2The performance map of/GO binary composite photocatalyst material degradation RhB；
Fig. 2 is MoS2、5wt%MoS2/GO、3wt%MoS2/GO/g-C3N4Scanning electron microscope (SEM) photograph and 3wt%MoS2/GO/g-C3N4's
Electronic dispersion energy map；
Fig. 3 is g-C3N4、MoS2、5wt%MoS2The MoS prepared in/GO and embodiment 2-42/GO/g-C3N4Diffusing reflection spectrum；
Fig. 4 is g-C3N4With the MoS prepared in embodiment 2-42/GO/g-C3N4Three-way catalyst photocatalytic degradation RhB performance map.
Specific embodiment
The present invention is described in further details below with reference to embodiment.Material therefor, reagent etc. are such as without spy in embodiment
Different explanation, is commercially available.
Embodiment 1:
The present invention is by first confirming MoS2The optimum catalyst ratio of/GO binary composite photocatalyst material synthesizes MoS in turn2/GO/
g-C3N4Tri compound catalysis material.With 5wt%MoS2For the preparation of/GO binary tri compound catalysis material:
By the MoO of 0.1439g3It is added in the deionized water of 10mL with the KSCN of 0.2429g, after stirring, ultrasonic disperse 30min
Obtain mixed solution；It disperses the GO of 0.005g in 10mL ethylene glycol, is add to the above mixed solution after being uniformly dispersed, after
Continuous ultrasonic disperse 30min, is fitted into 25mL reaction kettle, 180oConstant temperature is for 24 hours in the baking oven of C.With ethyl alcohol and going after being cooled to room temperature
Ionized water washs 3 times respectively, and centrifugation drying obtains the MoS that GO accounting is 5wt%2The binary composite photocatalyst material of/GO.
Wherein, the present invention is not particularly limited the specific source of the GO, can be commercially available or using Hummers oxidation
In addition method can also be used Brodie method, Staudenmaier method or Tour method and prepare.
Be respectively 0.001g with quality by above-mentioned preparation method, 0.003, the GO of 0.007g is prepared GO and accounts for MoS2/
GO gross mass is respectively 1%, 3%, 7% MoS2/ GO binary composite photocatalyst material；By the MoS of obtained different proportion2/ GO bis-
First composite photocatalyst material carries out the degradation experiment to RhB, degradation results as shown in Figure 1, difference GO accounting MoS2/ GO binary
Composite photocatalyst material is different to the catalytic performance of RhB degradation under visible light illumination；The result shows that the introducing of GO can improve
MoS2To the degradation efficiency of RhB, when GO content is 5wt%, degradation effect is best, this optimum proportioning is used for following each implementations
In example.
Embodiment 2
1wt%MoS2/GO/g-C3N4The preparation of tri compound catalysis material
The 5wt%MoS that will be prepared in 0.001g embodiment 12The g-C of/GO and 0.099g3N4It is added in the ethylene glycol of 20mL,
It is fitted into kettle after stirring and each 30min of ultrasonic disperse and is put into constant temperature in 180 DEG C of baking oven and for 24 hours, be cooled to room after the reaction was completed
Wen Houyong water and ethyl alcohol wash 3 times respectively, and MoS is made after centrifugation drying2/ GO accounting is the MoS of 1wt%2/GO/g-C3N4Three
First composite photocatalyst material.
Wherein, the present invention is to the g-C3N4Specific source be not particularly limited, can for it is commercially available or use solid phase reaction
Method, solvent-thermal method or thermal polymerization prepare.Preferably, the g-C3N4 is used following preparation method, specifically:
6g dicyanodiamine is placed in tube furnace, in a nitrogen atmosphere, with 5oC/min is kept from room temperature to 350 DEG C
120min, then with 5oC/min is warming up to 600 DEG C, keeps 120min, obtains g-C after cooling grinding3N4。
Embodiment 3
3wt%MoS2/GO/g-C3N4The preparation of tri compound catalysis material
The 5wt%MoS that will be prepared in 0.003g embodiment 22The g-C of/GO and 0.097g3N4It is added in the ethylene glycol of 20mL,
It is fitted into kettle after stirring and each 30min of ultrasonic disperse and is put into constant temperature in 180 DEG C of baking oven and for 24 hours, be cooled to room after the reaction was completed
Wen Houyong water and ethyl alcohol wash 3 times respectively, and MoS is made after centrifugation drying2/ GO accounting is the MoS of 3wt%2/GO/g-C3N4Three
First composite photocatalyst material.
Attached drawing 2 is MoS2、5wt%MoS2/GO、3wt%MoS2/GO/g-C3N4Scanning electron microscope (SEM) photograph and 3wt%MoS2/GO/g-
C3N4Electronic dispersion energy spectrum diagram；(A) is MoS in figure2Scanning electron microscope (SEM) photograph, (B) be 5wt%MoS2The scanning electron microscope (SEM) photograph of/GO,
It (C) is 3wt%MoS2/GO/g-C3N4Scanning electron microscope (SEM) photograph.As shown in figure, 3wt%MoS2/GO/g-C3N4Middle MoS2With smaller
Nanoscale and be dispersed on GO, and GO then with carrier material g-C3N4Under the action of π-is pi-conjugated combine it is even closer,
With MoS2And 5wt%MoS2/ GO is compared, MoS2Become smaller in size the introducing for illustrating GO and its and g-C3N4Synergistic effect can be with
Effective anchoring MoS2And the effect for limiting its growth is reached, this structure can effectively increase active site, but also electronics
Transmission rate is higher.It (D) is 3wt%MoS2/GO/g-C3N4Electronic dispersion energy map (EDS), it can be seen that C, N in map, O,
Mo, S element all exist, and further demonstrate the successful preparation of tri compound catalysis material, because EDS sample is drop in silicon wafer
The sample of upper system, so also occurring higher Si element peak in map.
Embodiment 4
5wt%MoS2/GO/g-C3N4The preparation of tri compound catalysis material
The 5wt%MoS that will be prepared in 0.005g embodiment 22The g-C of/GO and 0.095g3N4It is added in the ethylene glycol of 20mL,
It is fitted into kettle after stirring and each 30min of ultrasonic disperse and is put into constant temperature in 180 DEG C of baking oven and for 24 hours, be cooled to room after the reaction was completed
Wen Houyong water and ethyl alcohol wash 3 times respectively, and MoS is made after centrifugation drying2/ GO accounting is the MoS of 5wt%2/GO/g-C3N4Three
First composite photocatalyst material.
Fig. 3 is g-C3N4、MoS2、5wt%MoS2The MoS prepared in/GO and embodiment 2-42/GO/g-C3N4Diffuse
It composes (DRS)；As shown in figure, MoS2/GO/g-C3N4Tri compound catalysis material is relative to g-C3N4Photon absorbing intensity increase,
MoS2After/GO is introduced into, variation takes place in the ABSORPTION EDGE of tri compound catalysis material, works as MoS2The additive amount of/GO is 3wt%
When, ABSORPTION EDGE can be extended to about 580nm, hence it is evident that improve catalyst to the absorption region of visible light.
Embodiment 5
1wt%MoS2/GO/g-C3N4Tri compound catalysis material is used for visible light photocatalytic degradation RhB
(1) 0.050g1wt%MoS is weighed2/GO/g-C3N4Catalysis material be placed in 100mL light reaction bottle, and be added
50mLRhB aqueous solution (10mg/L), light reaction bottle is placed in light reaction instrument；
(2) it is passed through air in phototropic reaction bottle, magnetic agitation 30min makes reaction system reach adsorption-desorption under dark condition
Balance；
(3) light source (xenon lamp λ > 400nm of 300W) is opened, extract 5mL sample every 10min and be centrifuged；
(4) supernatant in (3) is taken to use liquid ultraviolet-uisible spectrophotometer (UV-2450) in wavelength 553nm in cuvette
Lower measurement, the variation of recording solution absorbance.
Embodiment 6
3wt%MoS2/GO/g-C3N4Tri compound catalysis material is used for visible light photocatalytic degradation RhB
(1) 0.050g3wt%MoS is weighed2/GO/g-C3N4Catalysis material be placed in 100mL light reaction bottle, and be added
50mLRhB aqueous solution (10mg/L), light reaction bottle is placed in light reaction instrument；
Step (2) (3) (4) is the same as embodiment 5.
Embodiment 7
5wt%MoS2/GO/g-C3N4Tri compound catalysis material is used for visible light photocatalytic degradation RhB:
(1) 0.050g5wt%MoS is weighed2/GO/g-C3N4Catalysis material be placed in 100mL light reaction bottle, and be added
50mLRhB aqueous solution (10mg/L), light reaction bottle is placed in light reaction instrument；
Step (2) (3) (4) is the same as embodiment 5.
The solution absorbance of 1 embodiment 5-7 of table changes
Attached drawing 4, Fig. 4 g-C are depicted as by the data in table 13N4With the MoS prepared in embodiment 2-42/GO/g-C3N4Ternary
Composite photocatalyst material degradation RhB performance map.As shown in figure, MoS2/GO/g-C3N4Tri compound catalysis material, which has, to be better than
Single MoS2、g-C3N4And binary MoS2The catalytic performance of/GO, in MoS2/ GO proportion is the MoS of 3wt%2/GO/g-C3N4
The catalytic degradation effect of tri compound catalysis material is best.After radiation of visible light 5h, 3wt%MoS2/GO/g-C3N4Degradation
The degradation rate of RhB is up to 96.7%, 5wt%MoS2/GO/g-C3N4The degradation rate of degradation RhB is 91.0%.As it can be seen that the present invention is mentioned
The MoS of confession2/GO/g-C3N4Tri compound catalysis material is relative to MoS2Or g-C3N4Monomer and MoS2/ GO binary is compound to urge
Agent all has the performance of more preferably photocatalytic degradation RhB, solar energy conversion and in terms of have and good answer
With prospect and economic benefit.
Claims (10)
1. a kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material, which is characterized in that the ternary is multiple
Light combination catalysis material is by MoS2/ GO binary composite and g-C3N4It is combined, wherein GO accounts for MoS2The 1 of/GO gross mass ~
7%；MoS2/ GO accounts for MoS2/GO/g-C3N4The 1 ~ 5% of tri compound catalysis material gross mass.
2. a kind of visible-light response type MoS as described in claim 12/GO/g-C3N4Tri compound catalysis material, feature
It is, GO accounts for MoS in the tri compound catalysis material2The 5% of/GO gross mass；MoS2/ GO accounts for MoS2/GO/g-C3N4Ternary
The 3 ~ 5% of composite photocatalyst material gross mass.
3. a kind of visible-light response type MoS as described in claim 12/GO/g-C3N4The preparation of tri compound catalysis material
Method, which comprises the following steps:
(1) by MoO3It is added in deionized water after stirring, ultrasonic disperse with KSCN and obtains mixed solution, disperse ethylene glycol for GO
It is added after solution in above-mentioned mixed solution, baking oven reaction is fitted into kettle and be put into after continuing ultrasonic disperse, is cooled down after the reaction was completed
To room temperature, MoS is prepared after centrifugation drying in washing2/ GO binary composite photocatalyst material；
(2) respectively by MoS obtained in above-mentioned steps (1)2/ GO binary composite photocatalyst material, g-C3N4It is added in ethylene glycol
Solution is fitted into reaction kettle to after even stirring, ultrasonic disperse and is put into baking oven reaction, is cooled to room temperature, washs after the reaction was completed,
MoS is prepared2/GO/g-C3N4Tri compound catalysis material.
4. preparation method according to claim 3, which is characterized in that MoO described in above-mentioned steps (1)3With rubbing for KSCN
You are than being 1:2.5.
5. preparation method according to claim 3, which is characterized in that GO and MoO described in above-mentioned steps (1)3Quality
Than for 1 ~ 7:144.
6. preparation method according to claim 3, which is characterized in that GO described in above-mentioned steps (1) and ethylene glycol
Proportionate relationship is 0.001 ~ 0.007g:10mL.
7. preparation method according to claim 3, which is characterized in that MoS described in above-mentioned steps (2)2/ GO and second two
The proportionate relationship of alcohol is than 0.001 ~ 0.005g:20mL.
8. preparation method according to claim 3, which is characterized in that MoS described in above-mentioned steps (2)2/ GO and g-
C3N4Mass ratio be 1:99 ~ 5:95.
9. preparation method according to claim 3, which is characterized in that in the step (1), (2), the baking oven reaction
To be reacted for 24 hours at 180 DEG C of temperature.
10. a kind of visible-light response type MoS according to claim 22/GO/g-C3N4Tri compound catalysis material,
It is characterized in that, the tri compound catalysis material is to concentration after radiation of visible light 5h for rhodamine B degradation
The degradation rate of the rhodamine B of 10mg/L reaches 91.0 ~ 96.7%.
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| CN111097477A (en) * | 2020-01-16 | 2020-05-05 | 兰州大学 | Preparation and application of ultrathin two-dimensional layered composite photocatalytic material |
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| CN111097477A (en) * | 2020-01-16 | 2020-05-05 | 兰州大学 | Preparation and application of ultrathin two-dimensional layered composite photocatalytic material |
| CN111097477B (en) * | 2020-01-16 | 2022-04-12 | 兰州大学 | Preparation and application of ultrathin two-dimensional layered composite photocatalytic material |
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