CN107096548A - A kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst and preparation method and application - Google Patents
A kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst and preparation method and application Download PDFInfo
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- CN107096548A CN107096548A CN201710393296.1A CN201710393296A CN107096548A CN 107096548 A CN107096548 A CN 107096548A CN 201710393296 A CN201710393296 A CN 201710393296A CN 107096548 A CN107096548 A CN 107096548A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 51
- 239000002127 nanobelt Substances 0.000 title claims abstract description 51
- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- 239000002096 quantum dot Substances 0.000 title claims abstract description 44
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 27
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 24
- 238000013019 agitation Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000003960 organic solvent Substances 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- 238000007146 photocatalysis Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 7
- 229910009891 LiAc Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- -1 molybdate dihydrate acid Chemical class 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims 4
- AQRDGTBNWBTFKJ-UHFFFAOYSA-N molybdenum;dihydrate Chemical compound O.O.[Mo] AQRDGTBNWBTFKJ-UHFFFAOYSA-N 0.000 claims 1
- 238000003776 cleavage reaction Methods 0.000 abstract description 13
- 230000007017 scission Effects 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
It is by TiO the invention discloses a kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst2Nanobelt and in its surface uniform load MoS2Quantum dot is constituted, wherein by quality ratio, MoS2:TiO2=0.1%~10%.The invention also discloses the preparation method of the photochemical catalyst and application, it is experimentally confirmed that the photochemical catalyst of the present invention has excellent photocatalytic cleavage water H2-producing capacity, in 30~120mW/cm2Radiation of visible light intensity, irradiation time is unit area (1m in the range of 0.1~8h2) photocatalytic cleavage water hydrogen-producing speed about 2.2mmol/h, simultaneously under sunshine, there is the ultraviolet light in sunshine humidification and quantum dot to strengthen the characteristic of light absorbs to photocatalytic cleavage water H2-producing capacity, make application broader, it is easy to spread, with great application value.
Description
Technical field
The present invention relates to a kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst and its preparation
Method and application；Belong to catalysis material technical field.
Background technology
Titanium dioxide is a kind of efficient photolytic hydrogen production catalyst, is urged always as a kind of most important light from 1981
Agent is widely studied by people.Heterojunction structure photochemical catalyst is to be used to strengthen one of photocatalysis effective way.Heterojunction photocatalysis
Agent is often any more single-phase with more preferable catalytic performance in heterojunction structure than constituting.In order to improve Photocatalyzed Hydrogen Production performance, people
Carried out substantial amounts of research work.Wherein, it is to improve the most important hand of photocatalysis performance to improve photo-generated carrier separating capacity
One of section.In order to improve TiO2Photochemical catalyst carrier separation ability, people usually form different using rutile-anatase two-phase
Matter structure, high efficiency photocatalysis is realized using interface band engineering.But isomerism hetero-junctions promotes carrier separation to have one
Fixed limitation, regulation and control difficulty is big, and cost is high, it is difficult to realize mass.Therefore, by TiO2Surface self-organization is specifically helped
Catalyst may make up catalytic active center, and H is produced to promote splitting water to react2Or O2.Common co-catalyst such as Au, Pt and
The noble metals such as Pd, narrow band gap metal oxide or sulfide are widely used in producing H2, but the activated centre that noble metal is constituted, into
This height, is equally difficult to mass, carries out practical application.In order to overcome these to challenge, non precious metal catalysis is gradually entered
One step develops, in non precious metal catalysis, transient metal sulfide nano material, such as MoS2Deng due to unique photo electric
Matter and receive great attention.
Class graphene two dimension MoS2With anisotropy, chemical inertness, electric conductivity, fast light corrosion and excellent photoelectric characteristic etc.
And be widely studied.On stratiform class graphene MoS2/TiO2Composite photocatalyst nano material is in photocatalytic cleavage aquatic products hydrogen or light
Research work in terms of catalytic degradation organic pollution has been reported.But through retrieval, so far, on MoS2Quantum dot/
Superfine Ti O2Hetero-junctions nanobelt photochemical catalyst, especially with TiO2Nanobelt is matrix, and area load has MoS2Quantum dot
MoS2/TiO2Hetero-junctions and its application in terms of photocatalytic cleavage aquatic products hydrogen have no report.
The content of the invention
Cost height, photocatalysis big extensively using difficulty are prepared for the reproducible hydrogen energy source of environment-protecting clean in the prior art
Agent efficiency is low and there is the deficiencies such as potential secondary pollution, and the problem to be solved in the present invention is to provide a kind of molybdenum disulfide quantum
Point/superfine titanic oxide hetero-junctions nanobelt and preparation method and application.
Molybdenum disulfide quantum dot of the present invention/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst, its feature exists
In：The catalyst is by a length of 200nm~400nm of size, and a width of 10nm-20nm, thickness is 3nm-8nm TiO2Nanobelt and
The MoS for being 5nm ± 2nm in the particle size of its surface uniform load2Quantum dot is constituted, wherein by quality ratio, MoS2:TiO2
=0.1%~10%.
Wherein：The catalyst is preferably by a length of 250nm~350nm of size, and a width of 10nm-18nm, thickness is 3nm-6nm
TiO2Nanobelt and its surface uniform load particle size be 5nm ± 2nm MoS2Quantum dot is constituted, wherein with quality
Than meter, MoS2:TiO2=1%~6%.
The preparation method of molybdenum disulfide quantum dot of the present invention/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst,
Step is：
1. N,N-dimethylformamide by volume:Glacial acetic acid (DMF:HAc)=6:4 prepare mixed organic solvents, then
It is blended with machine solvent, LiAc2H2O, butyl titanate is added sequentially in hydrothermal reaction kettle by setting ratio, compactedness control
System stirs the 50%~80% of reactor volume；Then hydrothermal reaction kettle is sealed, is put it into drying box, is made
Hydrothermal temperature control is at 200 ± 10 DEG C, and reaction time control naturally cools to room temperature, gained in 16h~24h, reaction after terminating
Product is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, is dried, and obtained white powder is superfine Ti O2Nanobelt；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, is prepared concentration and is
0.5g//L~5g/L TiO2Suspension, resulting solution is labeled as solution A；
3. MoS in mass ratio2:TiO2=0.5%~10% ratio, under the conditions of ultrasonic agitation, is added into solution A
The mol ratio of the Sodium Molybdate Dihydrate and thiocarbamide of respective reaction amount, wherein molybdate dihydrate acid and thiocarbamide is 2:1~1:8, continue ultrasound and stir
60 ± 5min is mixed, resulting solution is labeled as B solution；
4. obtained B solution is added in hydrothermal reaction kettle, compactedness is controlled the 50%~80% of reactor volume,
Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction time control exists
16h~24h, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed repeatedly with deionized water, then suction filtration, dries, i.e.,
Obtain molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
In the preparation method of above-mentioned molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst：Step
1. the mixed organic solvents, LiAc2H2O, butyl titanate preferably presses 100L mixed organic solvents, 2000g LiAc
2H2The ratio of O, 20L butyl titanate is added sequentially in hydrothermal reaction kettle.
In the preparation method of above-mentioned molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst：Step
2. the TiO2The concentration of suspension is preferably 1g//L~3g/L.
In the preparation method of above-mentioned molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst：Step
3. the mol ratio of the molybdate dihydrate acid and thiocarbamide is preferably 1:2.
Molybdenum disulfide quantum dot of the present invention/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst is in photocatalytic cleavage
Water prepares the application in hydrogen energy source.
Experiment display：Using molybdenum disulfide quantum dot of the present invention/superfine titanic oxide hetero-junctions nanobelt photocatalysis
Agent unit area (1m2) photocatalytic cleavage water hydrogen-producing speed about 2.2mmol/h；Wherein：The bar of the photocatalytic cleavage water hydrogen manufacturing
Part is：Spectral region is full spectrum sunshine, 30~120mW/cm of photo-irradiation intensity2, irradiation time is 0.1~8h.
The invention discloses a kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst, the light
Catalyst is under the conditions of sunshine irradiation, and with excellent photocatalytic cleavage water H2-producing capacity, improve sunshine utilizes effect
Rate, practical application is convenient, flexible, solves photochemical catalyst cost height, the low problem of efficiency.
The present invention is prepared for molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photocatalysis using hydro-thermal method
Agent.The photochemical catalyst is with superfine Ti O2Nanobelt is matrix, the uniform MoS of area load2Quantum dot is constituted, wherein ultra-fine
TiO2Nanobelt and MoS2The mass ratio of quantum dot is MoS2:TiO2=0.5%~10%.It is experimentally confirmed that the photocatalysis of the present invention
Agent has excellent photocatalytic cleavage water H2-producing capacity, in 30~120mW/cm2Radiation of visible light intensity, irradiation time is 0.1
Unit area (1m in the range of~8h2) photocatalytic cleavage water hydrogen-producing speed about 2.2mmol/h, while under sunshine, sunshine
In ultraviolet light there is humidification and quantum dot to strengthen the characteristic of light absorbs to photocatalytic cleavage water H2-producing capacity, make application
Scope is broader, it is easy to promote, with great application value.
Brief description of the drawings
Fig. 1 is the molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst ESEM prepared
(SEM) photo.
Fig. 2 divides for the molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst EDS elements prepared
Analysis.
Fig. 3 is the molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst transmission electron microscope prepared
(TEM) photo.
Fig. 4 is the molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst prepared in solar irradiation
Penetrate lower splitting water hydrogen-producing speed curve map.
Embodiment
Embodiment 1：
1. N,N-dimethylformamide by volume:Glacial acetic acid (DMF:HAc)=6:4 prepare mixed organic solvents, then
It is blended with machine solvent, LiAc2H2O, butyl titanate presses 100L mixed organic solvents, 2000g LiAc2H2O, 20L titanium
The ratio of sour four butyl esters is added sequentially in hydrothermal reaction kettle, and compactedness is controlled the 60% of reactor volume, and is stirred；
Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 DEG C, the reaction time is controlled in 20h,
Reaction naturally cools to room temperature after terminating, products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, dries, obtain
White powder be superfine Ti O2Nanobelt；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and preparation concentration is 1g/L
TiO2Suspension, resulting solution is labeled as solution A；
3. MoS in mass ratio2:TiO2=2% ratio, under the conditions of ultrasonic agitation, respective reaction is added into solution A
The mol ratio of the Sodium Molybdate Dihydrate and thiocarbamide of amount, wherein molybdate dihydrate acid and thiocarbamide is 1:2, continue ultrasonic agitation 60min, gained is molten
Liquid is labeled as B solution；
4. obtained B solution is added in hydrothermal reaction kettle, compactedness controls 60%, the Ran Houmi in reactor volume
Hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control at 200 DEG C, reaction time control is in 20h, reaction knot
Room temperature is naturally cooled to after beam, products therefrom is rinsed repeatedly with deionized water, then suction filtration, dry, that is, obtain molybdenum disulfide amount
Sub- point/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
Molybdenum disulfide quantum dot obtained above/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst is reflected as follows
Fixed and detection：
By the molybdenum disulfide quantum dot of gained/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst sample FDAC
Company's production HITACHI S-4800 types field emission scanning electron microscopes (SEM) are observed (result is shown in Fig. 1), ESEM
Provisioned EDS elementary analysis results are shown in Fig. 2.
By the molybdenum disulfide quantum dot of gained/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst sample JEOL
Company's production JEOL 2100F projection electron microscopes are observed (result is shown in Fig. 3).
Obtained photocatalytic cleavage water paper is implemented under visible light illumination to carry out splitting water H2-producing capacity to deionized water
Detection, in 100mW/cm2Radiation of visible light intensity, irradiation time be 0.1~8h in the range of, unit area (1m2) photocatalysis splits
Solve water hydrogen-producing speed about 2.2mmol/h (result is shown in Fig. 4).
Embodiment 2：
1. by volume ratio DMF:HAc (N,N-dimethylformamides：Glacial acetic acid)=6:4 mixed organic solvents, LiAc
2H2O, butyl titanate presses 120L mixed organic solvents, 2100g LiAc2H2The ratio of O, 25L butyl titanate is sequentially added
Into hydrothermal reaction kettle, compactedness is controlled the 50% of reactor volume, and is stirred；Then hydrothermal reaction kettle is sealed, will
It is put into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction time control terminates rear natural cooling in 16h, reaction
To room temperature, products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, dries, obtain superfine Ti O2Nanobelt white
Powder；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and obtained concentration is
0.5g//L TiO2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=0.5% ratio, under the conditions of ultrasonic agitation, into solution A in molar ratio 2：1
The Sodium Molybdate Dihydrate and thiocarbamide of respective reaction amount are added, and continues 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% of reactor volume, then seals hydro-thermal
Reactor, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, the reaction time is controlled in 16h, and reaction terminates
After naturally cool to room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, dry, obtain molybdenum disulfide quantum dot/
Superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
Embodiment 3：
1. by volume ratio DMF:HAc (N,N-dimethylformamides：Glacial acetic acid)=6:4 mixed organic solvents, LiAc
2H2O, butyl titanate presses 100L mixed organic solvents, 2000g LiAc2H2The ratio of O, 20L butyl titanate is sequentially added
Into hydrothermal reaction kettle, compactedness is controlled the 70% of reactor volume, and is stirred；Then hydrothermal reaction kettle is sealed, will
It is put into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction time control terminates rear natural cooling in 18h, reaction
To room temperature, products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, dries, obtain superfine Ti O2Nanobelt white
Powder；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and it is 3g/L that concentration, which is made,
TiO2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=4% ratio, under the conditions of ultrasonic agitation, into solution A in molar ratio 1：1 adds
Enter the Sodium Molybdate Dihydrate and thiocarbamide of respective reaction 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, the reaction time is controlled in 18h, and reaction terminates
After naturally cool to room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, dry, obtain molybdenum disulfide quantum dot/
Superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
Embodiment 4：
1. by volume ratio DMF:HAc (N,N-dimethylformamides：Glacial acetic acid)=6:4 mixed organic solvents, LiAc
2H2O, butyl titanate is added sequentially in hydrothermal reaction kettle, and compactedness control stirs equal the 75% of reactor volume
It is even；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydrothermal temperature control in 200 ± 10 DEG C, reaction time control
In 22h, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, does
It is dry, obtain superfine Ti O2Nanobelt white powder；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and it is 4g//L that concentration, which is made,
TiO2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=8% ratio, under the conditions of ultrasonic agitation, into solution A in molar ratio 1：4 add
Enter the Sodium Molybdate Dihydrate and thiocarbamide of respective reaction 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 75% of reactor volume, then seals hydro-thermal
Reactor, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, the reaction time is controlled in 22h, and reaction terminates
After naturally cool to room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, dry, obtain molybdenum disulfide quantum dot/
Superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
Embodiment 5：
1. by volume ratio DMF:HAc (N,N-dimethylformamides：Glacial acetic acid)=6:4 mixed organic solvents, LiAc
2H2O, butyl titanate presses 100L mixed organic solvents, 2000g LiAc2H2The ratio of O, 20L butyl titanate is sequentially added
Into hydrothermal reaction kettle, compactedness is controlled the 80% of reactor volume, and is stirred；Then hydrothermal reaction kettle is sealed, will
It is put into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, reaction time control terminates rear natural cooling in 24h, reaction
To room temperature, products therefrom is rinsed to neutrality repeatedly with absolute ethyl alcohol, and then suction filtration, dries, obtain superfine Ti O2Nanobelt white
Powder；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and it is 5g/L that concentration, which is made,
TiO2Suspension, resulting solution is labeled as A；
3. MoS in mass ratio2:TiO2=10% ratio, under the conditions of ultrasonic agitation, into solution A in molar ratio 1：8
The Sodium Molybdate Dihydrate and thiocarbamide of respective reaction amount are added, and continues 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is added in hydrothermal reaction kettle, compactedness is controlled the 80% of reactor volume, then seals hydro-thermal
Reactor, puts it into drying box, makes hydrothermal temperature control at 200 ± 10 DEG C, the reaction time is controlled in 24h, and reaction terminates
After naturally cool to room temperature, products therefrom is rinsed repeatedly with deionized water, then suction filtration, dry, obtain molybdenum disulfide quantum dot/
Superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
Claims (7)
1. a kind of molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst, it is characterised in that：The catalysis
Agent is by a length of 200nm~400nm of size, and a width of 10nm-20nm, thickness is 3nm-8nm TiO2Nanobelt and equal on its surface
The particle size of even load is 5nm ± 2nm MoS2Quantum dot is constituted, wherein by quality ratio, MoS2:TiO2=0.1%~
10%.
2. molybdenum disulfide quantum dot as claimed in claim 1/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst, its feature
It is：The catalyst is by a length of 250nm~350nm of size, and a width of 10nm-18nm, thickness is 3nm-6nm TiO2Nanobelt
The MoS for being 5nm ± 2nm with the particle size in its surface uniform load2Quantum dot is constituted, wherein by quality ratio, MoS2:
TiO2=1%~6%.
3. the preparation side of molybdenum disulfide quantum dot described in claim 1 or 2/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst
Method, step is：
1. N,N-dimethylformamide by volume:Glacial acetic acid (DMF:HAc)=6:4 prepare mixed organic solvents, then will be mixed
Close organic solvent, LiAc2H2O, butyl titanate is added sequentially in hydrothermal reaction kettle by setting ratio, and compactedness control exists
The 50%~80% of reactor volume, and stir；Then hydrothermal reaction kettle is sealed, is put it into drying box, makes hydro-thermal
Temperature control is at 200 ± 10 DEG C, and reaction time control naturally cools to room temperature, products therefrom in 16h~24h, reaction after terminating
Rinsed repeatedly with absolute ethyl alcohol to neutrality, then suction filtration, is dried, obtained white powder is superfine Ti O2Nanobelt；
2. the TiO for taking step 1. to obtain2Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, preparation concentration be 0.5g//L~
5g/L TiO2Suspension, resulting solution is labeled as solution A；
3. MoS in mass ratio2:TiO2=0.5%~10% ratio, under the conditions of ultrasonic agitation, is added corresponding into solution A
The mol ratio of the Sodium Molybdate Dihydrate and thiocarbamide of reacting dose, wherein molybdate dihydrate acid and thiocarbamide is 2:1~1:8, continue ultrasonic agitation 60
± 5min, resulting solution is labeled as B solution；
4. obtained B solution is added in hydrothermal reaction kettle, compactedness control is the 50%~80% of reactor volume, then
Seal hydrothermal reaction kettle, put it into drying box, make hydrothermal temperature control at 200 ± 10 DEG C, reaction time control 16h~
24h, reaction naturally cools to room temperature after terminating, and products therefrom is rinsed repeatedly with deionized water, then suction filtration, dries, that is, obtains
Molybdenum disulfide quantum dot/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst.
4. the preparation side of molybdenum disulfide quantum dot as claimed in claim 3/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst
Method, it is characterised in that：The step 1. mixed organic solvents, LiAc2H2O, butyl titanate by 100L mixed organic solvents,
2000g LiAc·2H2The ratio of O, 20L butyl titanate is added sequentially in hydrothermal reaction kettle.
5. the preparation side of molybdenum disulfide quantum dot as claimed in claim 3/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst
Method, it is characterised in that：The step 2. TiO2The concentration of suspension is 1g//L~3g/L.
6. the preparation side of molybdenum disulfide quantum dot as claimed in claim 3/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst
Method, it is characterised in that：3. the sour mol ratio with thiocarbamide of the molybdate dihydrate is 1 to step:2.
7. molybdenum disulfide quantum dot described in claim 1 or 2/superfine titanic oxide hetero-junctions nanobelt photochemical catalyst is in photocatalysis
Splitting water prepares the application in hydrogen energy source.
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Cited By (3)
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| CN107993923A (en) * | 2017-12-08 | 2018-05-04 | 青岛大学 | A kind of controllable quantum dots array preparation method based on photo-thermal effect |
| CN109967095A (en) * | 2019-04-17 | 2019-07-05 | 南昌航空大学 | A kind of holocrystalline bulk heterojunction catalysis material and its preparation method and application |
| CN110124701A (en) * | 2019-06-25 | 2019-08-16 | 泉州师范学院 | A kind of preparation method and applications of molybdenum disulfide quantum dot/titanium dioxide nanoplate composite photo-catalyst |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107993923A (en) * | 2017-12-08 | 2018-05-04 | 青岛大学 | A kind of controllable quantum dots array preparation method based on photo-thermal effect |
| CN107993923B (en) * | 2017-12-08 | 2020-02-21 | 青岛大学 | Preparation method of controllable quantum dot array based on photothermal effect |
| CN109967095A (en) * | 2019-04-17 | 2019-07-05 | 南昌航空大学 | A kind of holocrystalline bulk heterojunction catalysis material and its preparation method and application |
| CN109967095B (en) * | 2019-04-17 | 2021-05-25 | 南昌航空大学 | Full-crystal heterojunction photocatalytic material and preparation method and application thereof |
| CN110124701A (en) * | 2019-06-25 | 2019-08-16 | 泉州师范学院 | A kind of preparation method and applications of molybdenum disulfide quantum dot/titanium dioxide nanoplate composite photo-catalyst |
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