CN105597787B - A kind of individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst and preparation method thereof - Google Patents
A kind of individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst and preparation method thereof Download PDFInfo
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- CN105597787B CN105597787B CN201610096318.3A CN201610096318A CN105597787B CN 105597787 B CN105597787 B CN 105597787B CN 201610096318 A CN201610096318 A CN 201610096318A CN 105597787 B CN105597787 B CN 105597787B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000002127 nanobelt Substances 0.000 title claims abstract description 51
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 43
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 10
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 20
- 238000013019 agitation Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 9
- -1 thio ammonium molybdate Chemical compound 0.000 claims description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 6
- 239000011609 ammonium molybdate Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005286 illumination Methods 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 33
- 239000000463 material Substances 0.000 description 17
- 239000011941 photocatalyst Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 229910009891 LiAc Inorganic materials 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000000523 sample Substances 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000035800 maturation Effects 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- B01J35/39—
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
- A62D3/176—Ultraviolet radiations, i.e. radiation having a wavelength of about 3nm to 400nm
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/40—
-
- 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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/26—Organic substances containing nitrogen or phosphorus
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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
The invention discloses a kind of individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst, it is by a length of 100nm~300nm of size, the two-dimension nano materials MoS that a width of 5nm~15nm, superfine titanic oxide nanobelt that thickness is 1nm~5nm and the thickness that one layer is wrapped up on its surface are 0.8nm~3nm2Constitute, wherein, MoS. in the photochemical catalyst by quality ratio2:TiO2=0.1~10:100.The photochemical catalyst of the present invention combines MoS2And TiO2Property, on the one hand illumination effect under, MoS2Be conducive to carrier molecule, and the carrier produced promotes superfine Ti O2The light-catalyzed reaction activity of nanobelt, has good catalytic performance to the degraded and Photocatalyzed Hydrogen Production of organic contamination model thing；On the other hand the hetero-junctions can effectively suppress produced Carrier recombination.Photochemical catalyst synthesis technique of the present invention, equipment are simple, and cost is low, efficiency high, and reaction time is short, and reproducible, industrial applications have a extensive future.
Description
Technical field
The present invention relates to a kind of heterojunction structure photochemical catalyst and preparation method thereof, more particularly to a kind of individual layer molybdenum disulfide/
Superfine titanic oxide nanobelt (MoS2/TiO2) heterojunction structure photochemical catalyst and preparation method and application, belong to nano material light
Catalysis technical field.
Background technology
Photochemical catalyst is that one kind itself is not involved in reacting and accelerating photochemically reactive material.Photocatalysis is photochemistry with urging
The combination of agent.Under the overall background of environmental pollution and energy crisis, photocatalysis prepares clean energy resource-hydrogen and drop
It is a kind of high effective green environmentally friendly new technology developed in recent years to solve organic pollution.But its grinding as New function material
Hair, also faces many limitations, such as catalytic performance is single, and catalyst efficiency, inactivation and secondary pollution, sun light utilization efficiency are low
Deng.Based on this, exploitation and structure heterojunction structure turn into the important means of currently acquired novel high-performance catalysis material.
After graphene, molybdenum disulfide is the stratified nano materials for enjoying extensive concern.Individual layer molybdenum disulfide has excellent
Luminous efficiency more, excellent photon transport rate and itself chemical stability, has had in fields such as two-dimensional material electronics
Relatively broad deeply probes into, and it is that global scientist thinks that new generation semiconductor is quite potential to have scholarly forecast individual layer molybdenum disulfide
Material [HUANG Y L, CHEN Y, ZHANG W, et al.Bandgap tunability at single-layer
molybdenum disulphide grain boundaries[J].Nature communications,2015,6
(6298.]。
Titanium dioxide is the catalysis material of current more maturation, wherein nano titanium oxide P25, nano titania
Ball, nano flower, the nano material such as nanometer rods has good ultraviolet catalytic performance, the existing wide coverage of its photocatalysis performance.
But the catalysis material of even maturation still suffers from following shortcomings：High catalytic activity face exposes less, recovery separation is difficult, only
Excited under ultraviolet light conditions, sun light utilization efficiency is low.Superfine titanic oxide nanobelt equally only under ultraviolet light have compared with
High catalytic performance, but it has higher active face, the advantages of easily reclaiming.But so far, for individual layer curing
The heterojunction structure that molybdenum/superfine titanic oxide nanobelt is compounded to form, and utilize individual layer molybdenum disulfide and superfine titanic oxide nanometer
Had not been reported with heterojunction structure as application of the photochemical catalyst in catalyzing and degrading pollutant and production hydrogen.
The content of the invention
In view of the shortcomings of the prior art, the problem to be solved in the present invention be to provide it is a kind of have photocatalytic pollutant degradation with
And the individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS of production two kinds of performances of hydrogen2-TiO2) heterojunction structure photochemical catalyst and its
Preparation method and application.
Individual layer molybdenum disulfide of the present invention/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst, its feature exists
In：The photochemical catalyst is by a length of 100nm~300nm of size, and a width of 5nm~15nm, thickness is 1nm~5nm ultra-fine dioxy
Change titanium nanobelt and two-dimension nano materials MoS of one layer of the thickness for 0.8nm~3nm is wrapped up on its surface2Constitute, wherein described
In photochemical catalyst by quality ratio, MoS2:TiO2=0.1~10:100.
Above-mentioned individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst is preferred embodiment：
The photochemical catalyst is by a length of 200nm ± 50nm of size, and a width of 10nm ± 2nm, thickness is 3nm ± 1nm superfine titanic oxide
The two-dimension nano materials MoS that nanobelt and the thickness that one layer is wrapped up on its surface are 1nm ± 0.2nm2Constitute, wherein the light is urged
In agent by quality ratio, MoS2:TiO2=3~6:100, most preferably MoS2:TiO2=5:100.
The preparation method of individual layer molybdenum disulfide of the present invention/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst,
Step is：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions are mixed with
Machine solvent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc
2H2The proportional quantities of O, 2L butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 50% of reactor volume
~80%, and stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control 200 ± 10
DEG C, 16h~24h is reacted, reaction naturally cools to room temperature after terminating, products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, so
Suction filtration, drying afterwards, obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, 30 ± 5min of ultrasonic agitation, system
The TiO that standby concentration is 0.5g//L~5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=0.1~10:100 ratio, phase is added into solution A under the conditions of ultrasonic agitation
The four thio ammonium molybdate of reacting dose is answered, and continues 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness controls 50%~80%, the Ran Houmi in reactor volume
Hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 16h~24h, reaction terminates
After naturally cool to room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, and obtained solid powder is
Individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
In the preparation method of above-mentioned individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst：Step
3. the MoS2:TiO2Preferably 3~6:100, most preferably 5:100.
Individual layer molybdenum disulfide of the present invention/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst is in catalytic degradation
Application in pollutant and Photocatalyzed Hydrogen Production.
The present invention is prepared for individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS using hydro-thermal method2-TiO2) hetero-junctions
Structure photochemical catalyst, is obtained by superfine Ti O2Nanobelt and in its surface parcel two-dimension nano materials MoS2MoS2-TiO2Nanometer
Band heterojunction structure catalysis material.The efficient light absorption of individual layer molybdenum disulfide, excellent electron transfer are make use of in the present invention
Rate and both good chemical stability and the advantage of superfine nano titanium dioxide are compound, are successfully prepared individual layer curing
Molybdenum wraps up titanium dioxide nano-belts composite photo-catalyst, has good degradation effect and production hydrogen to methyl orange under sunshine
Performance.
Experiment is confirmed：The heterojunction structure photochemical catalyst of the present invention is with TiO2For matrix, area load has high catalytic activity
Two-dimension nano materials MoS2, combine excellent photochemical catalyst TiO2And the MoS of high photonic absorption, mobility2Property,
Under illumination effect, be conducive to carrier molecule, the carrier produced in addition promotes TiO2Light-catalyzed reaction activity.In light
According under the conditions of, there is good catalytic performance to the degraded and Photocatalyzed Hydrogen Production of organic contamination model thing.
Brief description of the drawings
Fig. 1 is the MoS prepared2、TiO2, individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) hetero-junctions
X-ray diffraction (XRD) collection of illustrative plates of structure photocatalyst material.
Fig. 2 is the individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS prepared2-TiO2) heterojunction structure photochemical catalyst
Transmission electron microscope (TEM) photo of material.
Fig. 3 is the individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS prepared2-TiO2) heterojunction structure photochemical catalyst
Photo under material transmission Electronic Speculum (TEM) high power.
Fig. 4 is individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photocatalyst material sweeps
Retouch transmission electron microscope (STEM) photo
Wherein：(a) individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS to prepare2-TiO2) heterojunction structure light urges
Scanning transmission electron microscope (STEM) photo of agent material, (b) is EDS mapping, and (c) is the partial enlargement TEM of STEM photos
Photo.
Fig. 5 is individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst is ultraviolet
Light, it is seen that the degraded figure under light illumination, and Photocatalyzed Hydrogen Production time history plot
Wherein：(a) the individual layer MoS with (b) to prepare2/ superfine Ti O2Nanobelt heterojunction structure photocatalyst material is ultraviolet
Light (a), it is seen that the degraded figure under light (b) illumination, (c) is Photocatalyzed Hydrogen Production time history plot.
Embodiment
Embodiment 1：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions are mixed with
Machine solvent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc
2H2The proportional quantities of O, 2L butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 50% of reactor volume
~80%, and stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control 200 ± 10
DEG C, 20h is reacted, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality, then taken out repeatedly with absolute ethyl alcohol
Filter, dry, obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, 30 ± 5min of ultrasonic agitation, system
The TiO that standby concentration is 3.5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=5:100 ratio, respective reaction is added into solution A under the conditions of ultrasonic agitation
The four thio ammonium molybdate of amount, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness controls 50%~80%, the Ran Houmi in reactor volume
Envelope hydrothermal reaction kettle, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 20h, reacts after terminating certainly
Room temperature so is cooled to, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, obtained solid powder as individual layer
Molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
By the MoS being related in embodiment2、TiO2, individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) different
Matter structure light catalyst sample Germany Brooker D8X- x ray diffractometer xs analysis (result is shown in Fig. 1).
By the individual layer MoS of gained2/ superfine Ti O2Nanobelt heterojunction structure photocatalyst material sample JEOL companies of Japan
Production JEM 2100F type transmission electron microscopes are observed (result is shown in Fig. 2, Fig. 3), and to catalyst member under dark field mode
Element is analyzed.Individual layer molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photocatalyst material
Scanning transmission electron microscope (STEM) photographic result is shown in Fig. 4.
By the individual layer MoS of gained2/ superfine Ti O2Nanobelt heterojunction structure photocatalyst material sample ultraviolet light (UV) and
Methyl orange is degraded under visible ray (Vis) irradiation, being degraded to 100% after being irradiated respectively through 15min, 120min, (result is shown in
Fig. 5 a and Fig. 5 b)；It is 75.0 μm of olg to measure the photocatalytic water hydrogen-producing speed under the conditions of simulated solar light irradiation simultaneously-1·h-1
(result is shown in Fig. 5 c).
Embodiment 2：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions are mixed with
Machine solvent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc
2H2The proportional quantities of O, 2L butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 60% of reactor volume
~80%, and stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control 200 ± 10
DEG C, 16h is reacted, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality, then taken out repeatedly with absolute ethyl alcohol
Filter, dry, obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, 30 ± 5min of ultrasonic agitation, system
The TiO that standby concentration is 1.5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=10:100 ratio, into solution A, addition is corresponding anti-under the conditions of ultrasonic agitation
The four thio ammonium molybdate that should be measured, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness controls 60%~80%, the Ran Houmi in reactor volume
Envelope hydrothermal reaction kettle, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 16h, reacts after terminating certainly
Room temperature so is cooled to, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, obtained solid powder as individual layer
Molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
Embodiment 3：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions are mixed with
Machine solvent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc
2H2The proportional quantities of O, 2L butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 60% of reactor volume
~70%, and stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control 200 ± 10
DEG C, 24h is reacted, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality, then taken out repeatedly with absolute ethyl alcohol
Filter, dry, obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, 30 ± 5min of ultrasonic agitation, system
The TiO that standby concentration is 4.5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=3:100 ratio, respective reaction is added into solution A under the conditions of ultrasonic agitation
The four thio ammonium molybdate of amount, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness controls 60%~70%, the Ran Houmi in reactor volume
Envelope hydrothermal reaction kettle, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 24h, reacts after terminating certainly
Room temperature so is cooled to, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, obtained solid powder as individual layer
Molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
Embodiment 4：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions are mixed with
Machine solvent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc
2H2The proportional quantities of O, 2L butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 70% of reactor volume,
And stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction
22h, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality, then suction filtration, drying repeatedly with absolute ethyl alcohol,
Obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, 30 ± 5min of ultrasonic agitation, system
The TiO that standby concentration is 5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=6:100 ratio, respective reaction is added into solution A under the conditions of ultrasonic agitation
The four thio ammonium molybdate of amount, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness is controlled the 70% of reactor volume, then seals hydro-thermal
Reactor, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 22h, reaction terminates rear natural cooling
To room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, and obtained solid powder is individual layer curing
Molybdenum/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
Claims (3)
1. a kind of preparation method of individual layer molybdenum disulfide/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst, step is：
1. with volume basis, by DMF:Glacial acetic acid (DMF:HAc)=6:4 proportions mixing is organic molten
Agent, by the mixed organic solvents, LiAc2H2O, butyl titanate press 10L mixed organic solvents, 200g LiAc2H2O, 2L
The proportional quantities of butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 50%~80% of reactor volume,
And stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction
16h~24h, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, then suction filtration,
Dry, obtained white powder is superfine titanic oxide nanobelt；
2. taking step, 1. obtained superfine titanic oxide nanobelt powder is dispersed in water, and 30 ± 5min of ultrasonic agitation is prepared dense
Spend the TiO for 0.5g//L~5g/L2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=0.1~10:100 ratio, into solution A, addition is corresponding anti-under the conditions of ultrasonic agitation
The four thio ammonium molybdate that should be measured, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness is controlled the 50%~80% of reactor volume, then seals water
Thermal response kettle, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reacts 16h~24h, reacts after terminating certainly
Room temperature so is cooled to, products therefrom is rinsed repeatedly with deionized water, then suction filtration, drying, obtained solid powder as individual layer
Molybdenum disulfide/superfine titanic oxide nanobelt (MoS2-TiO2) heterojunction structure photochemical catalyst.
2. the preparation side of individual layer molybdenum disulfide as claimed in claim 1/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst
Method, it is characterised in that：The step 3. MoS2:TiO2=3~6:100.
3. the preparation side of individual layer molybdenum disulfide as claimed in claim 2/superfine titanic oxide nanobelt heterojunction structure photochemical catalyst
Method, it is characterised in that：The step 3. MoS2:TiO2=5:100.
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| CN106423223B (en) * | 2016-09-20 | 2019-04-09 | 中国计量大学 | A kind of pie porous structure MoSe2@TiO2 photochemical catalyst and preparation method thereof |
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| CN107096548A (en) * | 2017-05-27 | 2017-08-29 | 青岛大学 | A kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst and preparation method and application |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402052A (en) * | 2014-10-30 | 2015-03-11 | 华东师范大学 | TiO2-quantum-dot-and-MoS2-nanometer-flower-combined heterojunction semiconductor material and preparation method thereof |
| CN105098151A (en) * | 2015-06-19 | 2015-11-25 | 上海交通大学 | Molybdenum disulfide-carbon hollow ball hybrid material and preparation method thereof |
| CN105148947A (en) * | 2015-08-27 | 2015-12-16 | 江南大学 | Preparation and application of TiO2@MoS2 composite |
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9527062B2 (en) * | 2013-05-09 | 2016-12-27 | North Carolina State University | Process for scalable synthesis of molybdenum disulfide monolayer and few-layer films |
-
2016
- 2016-02-22 CN CN201610096318.3A patent/CN105597787B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402052A (en) * | 2014-10-30 | 2015-03-11 | 华东师范大学 | TiO2-quantum-dot-and-MoS2-nanometer-flower-combined heterojunction semiconductor material and preparation method thereof |
| CN105098151A (en) * | 2015-06-19 | 2015-11-25 | 上海交通大学 | Molybdenum disulfide-carbon hollow ball hybrid material and preparation method thereof |
| CN105148947A (en) * | 2015-08-27 | 2015-12-16 | 江南大学 | Preparation and application of TiO2@MoS2 composite |
| CN105195133A (en) * | 2015-09-18 | 2015-12-30 | 黑龙江大学 | Preparation method of molybdenum disulfide-black titanium dioxide composite visible-light-driven photocatalyst for hydrogen production |
Non-Patent Citations (2)
| Title |
|---|
| Efficient synthesis of MoS2 nanoparticles modified TiO2 nanobelts with enhanced visible-light-driven photocatalytic activity;Hui Liu et al;《Journal of Molecular Catalysis A:Chemical》;20141012;第396卷;第136-142页 * |
| Synthesis of Few-Layer MoS2 Nanosheet-Coated TiO2 Nanobelt Heterostructures for Enhanced Photocatalytic Activities;Weijia Zhou et al;《small》;20121004;第9卷(第1期);第140-147页 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106799244A (en) * | 2017-01-10 | 2017-06-06 | 江苏大学 | The preparation method and purposes of a kind of Three-element composite photocatalyst |
| CN106799244B (en) * | 2017-01-10 | 2019-10-01 | 江苏大学 | A kind of preparation method and purposes of Three-element composite photocatalyst |
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