CN106902847A - A kind of molybdenum bisuphide/barium titanate ultrasound visible light catalyst and its preparation and application - Google Patents
A kind of molybdenum bisuphide/barium titanate ultrasound visible light catalyst and its preparation and application Download PDFInfo
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- CN106902847A CN106902847A CN201710183274.2A CN201710183274A CN106902847A CN 106902847 A CN106902847 A CN 106902847A CN 201710183274 A CN201710183274 A CN 201710183274A CN 106902847 A CN106902847 A CN 106902847A
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- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 26
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 26
- 239000011733 molybdenum Substances 0.000 title claims abstract description 26
- 238000002604 ultrasonography Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000035484 reaction time Effects 0.000 claims abstract description 16
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 15
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000004523 catalytic cracking Methods 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000013019 agitation Methods 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 7
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 7
- 229910001626 barium chloride Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000002525 ultrasonication Methods 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 150000004679 hydroxides Chemical class 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000003426 co-catalyst Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007233 catalytic pyrolysis Methods 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002389 environmental scanning electron microscopy 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
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method 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
-
- B01J35/39—
-
- B01J35/396—
-
- 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
-
- 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
-
- 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 molybdenum bisuphide/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst, be with size dimension as 80nm~barium titanate (BaTiO of 120nm3) nano cubic block is in 1~10 layer of molybdenum bisuphide (MoS that its area load thickness degree is 0.74~0.77nm2) be obtained；Wherein, with Ba/Mo molar ratio computings, Ba in the catalyst:Mo=5:1~100:1.Invention additionally discloses application of the catalyst in ultrasonic synergistic visible light catalytic cracking aquatic products hydrogen, catalyst of the present invention combines excellent visible light catalyst stratiform MoS2And BaTiO3Property, under ultrasonication, be conducive to carrier separation, and suppress compound, promote stratiform MoS2Visible light catalytic splitting water reactivity；Synthesis technique of the present invention and equipment are simple simultaneously, and low cost, efficiency high, reaction time are short, reproducible, and industrial applications have a extensive future.
Description
Technical field
The present invention relates to a kind of ultrasonic visible light catalyst and preparation method and application, more particularly to a kind of tool ultrasonic wave
Cooperate with the molybdenum bisuphide/barium titanate (MoS of visible light catalytic splitting water H2-producing capacity2/BaTiO3) nano cubic block heterojunction structure surpass
Sound visible light catalyst and preparation method and application；Belong to photocatalysis energy and material and its preparation field.
Background technology
Photocatalysis is a kind of photochemical reaction in the presence of a catalyst, is the combination of photochemistry and catalyst.Light
Catalytic pyrolysis aquatic products hydrogen is a kind of energy-conservation developed in recent years, high effective green environmentally friendly new technology.But it is used as New function
The research and development of material, also face many limitation, and such as catalytic efficiency is not high, sun light utilization efficiency is low, secondary pollution.
Heterojunction structure photochemical catalyst is for strengthening one of photocatalysis effective way.Heterojunction photocatalyst is often than constituting
Heterojunction structure it is any single-phase with more preferable catalytic performance.Therefore, suitable co-catalyst is selected, to build heterojunction structure light
Catalyst is the effective way for improving photocatalytic activity.Urged by be may make up in the specific co-catalyst of catalyst surface self assembly
Change activated centre, to promote to produce H to effective degraded of pollutant or splitting water reaction2Or O2.Common co-catalyst master
If noble metal such as Au, Ag, Pt and Pd etc. or specific metal oxide containing precious metals, it is widely used in producing H2, but actual industrial
It is restricted when in use.In addition to heterojunction structure can strengthen photocatalysis performance, using piezoelectric can realize mechanical energy with
The phenomenon that electric energy is exchanged；It is internal just to produce polarization i.e. when crystal is acted on by certain fixed-direction external force, while
The opposite electric charge of symbol is produced on certain two surface, built in field is formed；After external force is removed, crystal returns to uncharged again
State；When outer forced direction changes, the polarity of electric charge also changes therewith；The quantity of electric charge and external force produced by crystal stress
Size is directly proportional, therefore is likely to form one simultaneously and is influenceed transformable built in field by external force change, can be effectively promoted electricity
Lotus separates, and is remarkably improved photocatalysis performance.
BaTiO3Be it is well known that and the piezoelectric that is widely studied, it has the disadvantage separately as conductor photocatalysis
Agent is only issuing third contact of a total solar or lunar eclipse catalytic reaction in ultraviolet light conditions, and reaction efficiency is low, therefore its application is subject to certain restrictions.Through inspection
Rope, the correlative study report on ultrasonic wave added visible light catalytic splitting water is very few, especially with BaTiO3It is matrix, is coated with
Individual layer MoS2Photochemical catalyst and its application in terms of ultrasonic wave added visible light catalytic cracking aquatic products hydrogen have no report.
The content of the invention
In view of the shortcomings of the prior art, the problem to be solved in the present invention is to provide a kind of with supersonic synergic visible light catalytic
The molybdenum bisuphide of splitting water H2-producing capacity/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure ultrasound visible light catalyst
And preparation method and application.
Molybdenum bisuphide of the present invention/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst, its feature
It is：The catalyst be with size dimension as 80nm~barium titanate (BaTiO of 120nm3) nano cubic block is negative on its surface
Carrier layer thickness is 1~10 layer of molybdenum bisuphide (MoS of 0.74~0.77nm2) be obtained；Wherein, rubbed with Ba/Mo in the catalyst
You are than meter, Ba:Mo=5:1~100:1.
It is further it is preferable that：The catalyst is the barium titanate (BaTiO of ± 5nm with size dimension as 100nm3)
Nano cubic block is in 1~3 layer of molybdenum bisuphide (MoS that its area load thickness degree is 0.74~0.77nm2) be obtained；Wherein, institute
State in catalyst with Ba/Mo molar ratio computings, Ba:Mo=50:1~100:1；Most preferably Ba:Mo=50:1.
The preparation side of molybdenum bisuphide of the present invention/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst
Method, step is：
1. preparing BaTiO3Molar ratio computing, by mass ratio NaOH:KOH=51.5:48.5 anhydrous hydroxide,
BaCl2, nano-TiO2It is added sequentially in hydrothermal reaction kettle, compactedness control stirs equal the 40~80% of reactor volume
It is even；Then hydrothermal reaction kettle is sealed, is put it into drying box, hydrothermal temperature is controlled in 200 ± 10 DEG C, reaction time control
In 40h~60h, reaction naturally cools to room temperature after terminating, and products therefrom deionized water is rinsed to neutrality, then taken out repeatedly
Filter, dries, that is, obtain BaTiO3Powder；
2. the BaTiO that 1. step obtains is taken3Powder is simultaneously dispersed in water, 30 ± 5min of ultrasonic agitation, and compound concentration is
The BaTiO of 0.1g//L~2g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=5:1~100:1 ratio, under the conditions of ultrasonic agitation to solution A in add
Four or six generation ammonium molybdates (ATM) of respective reaction amount, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is poured into the high-temperature high-pressure reaction kettle equipped with polytetrafluoroethylene (PTFE), reactor is then inserted 200 ± 5
In DEG C baking oven, the reaction time is 24 ± 0.5h；Reaction terminates rear natural cooling and is down to room temperature, then through filtering, washing, 60 ± 5 DEG C
Under dry 12h, the dark gray powder for obtaining as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure surpass
Sound visible light catalyst.
Molybdenum bisuphide of the present invention/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst is assisted in ultrasonic wave
With the application in visible light catalytic cracking aquatic products hydrogen.
Experiment is confirmed：Under ultrasound condition, due to cavitation, when acting on the BaTiO with cube block structure3On
When, nanometer piezoelectric can be made to produce deformation.Because the crystal symmetry of nanometer piezoelectric is relatively low, sent out when being acted on by external force
During raw deformation, the relative displacement of negative ions makes positive and negative charge center no longer overlap in structure cell, causes crystal that macroscopic polarization occurs,
So that nanometer piezoelectric material surface produces opposite charges, promote the separation of carrier so that mechanical energy is converted into chemical energy, together
When again visible ray photograph in the presence of, further increase stratiform MoS2Photocatalytic cleavage aquatic products hydrogen activity.
The present invention is prepared for molybdenum bisuphide/barium titanate (MoS using the hot method of alkali and simple solvent-thermal method2/BaTiO3) receive
Rice cubic block heterojunction structure, obtains by BaTiO3Nano cubic block and the stratiform MoS in its area load2The curing of composition
Molybdenum/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure ultrasound visible light catalyst (wherein with Ba/Mo molar ratio computings,
Ba:Mo=5:1~100:1).The ultrasonic visible light catalyst is with piezoelectric BaTiO3It is matrix, area load is urged with height
Change the stratiform MoS of activity2, combine excellent visible light catalyst stratiform MoS2And BaTiO3Property, under ultrasonication,
Be conducive to carrier separation, and suppress compound, promote stratiform MoS2Visible light catalytic splitting water reactivity；While this hair
Bright synthesis technique and equipment are simple, and low cost, efficiency high, reaction time are short, reproducible, and photocatalytic cleavage aquatic products hydrogen application is easy
In realization and popularization, industrial applications have a extensive future.
Brief description of the drawings
Fig. 1 is the MoS for preparing2/BaTiO3ESEM (SEM) photo of nano cubic block composite.
Fig. 2 is the MoS for preparing2/BaTiO3Transmission electron microscope (TEM) photo of nano cubic block composite.
Fig. 3 is the MoS for preparing2/BaTiO3Nano cubic block composite is in ultrasound, illumination, supersonic synergic radiation of visible light
Lower splitting water H2-producing capacity curve map.
Specific embodiment
Embodiment 1：
1. by 20g anhydrous hydroxides (NaOH/KOH=51.5:48.5), 0.6mmol BaCl2, 0.5mmol nano-TiOs2
It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 40% of reactor volume, and is stirred；Then sealing hydro-thermal is anti-
Kettle is answered, is put it into drying box, hydrothermal temperature is controlled at 200 DEG C, reaction time control is in 40h, and reaction is natural after terminating
Room temperature is cooled to, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, dries, and obtains BaTiO3Powder；
2. the BaTiO that 1. step obtains is weighed3Powder 100mg, and be dispersed in 100mL water, ultrasonic agitation 30min is obtained
Concentration is the BaTiO of 1g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=50:1 ratio, under the conditions of ultrasonic agitation to solution A in add it is corresponding anti-
Four or the six generation ammonium molybdates (ATM) that should be measured, and continue ultrasonic agitation 60min, resulting solution is labeled as B；
4. B solution is poured into the high-temperature high-pressure reaction kettle equipped with polytetrafluoroethylene (PTFE), reactor is then inserted 200 ± 5
In DEG C baking oven, the reaction time is 24 ± 0.5h.Reaction terminates rear natural cooling and is down to room temperature, eventually passes filter, washing, 60 ± 5
12h is dried at DEG C, dark gray powder is obtained, as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure
Ultrasonic visible light catalyst.
By the MoS of gained2/BaTiO3Nano cubic block heterojunction structure ultrasound visible light catalyst sample Japan HITACHI
Production S-4800 type field emission scanning electron microscopes are observed (result is shown in Fig. 1).
By the MoS of gained2/BaTiO3Nano cubic block heterojunction structure ultrasound visible light catalyst sample is public with Japan JEOL
Department's production JEM 2100F type transmission electron microscopes are observed (result is shown in Fig. 2).
By the MoS of gained2/BaTiO3Nano cubic block heterojunction structure ultrasound visible light catalyst sample is respectively in ultrasound, light
According to splitting water H2-producing capacity test is carried out under, supersonic synergic light irradiation, supersonic synergic visible ray is as a result displayed under the conditions of, it is single
Position quality catalyst consumption (1g) catalytic pyrolysis water hydrogen-producing speed is at 0.1mmol/h (see Fig. 3).
Embodiment 2：
1. by 20g anhydrous hydroxides (NaOH/KOH=51.5:48.5), 0.6mmol BaCl2, 0.5mmol nano-TiOs2
It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 50% of reactor volume, and is stirred；Then sealing hydro-thermal is anti-
Kettle is answered, is put it into drying box, hydrothermal temperature is controlled at 200 DEG C, reaction time control is in 40h, and reaction is natural after terminating
Room temperature is cooled to, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, dries, and obtains BaTiO3Powder；
2. the BaTiO that 1. step obtains is weighed3Powder 100mg, and be dispersed in 100mL water, ultrasonic agitation 30min is obtained
Concentration is the BaTiO of 1.5g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=5:1 ratio, under the conditions of ultrasonic agitation to solution A in add respective reaction
Four or six generation ammonium molybdates (ATM) of amount, and continue ultrasonic agitation 60min, resulting solution is labeled as B；
4. during B solution is poured into equipped with polytetrafluoroethylene (PTFE) high-temperature high-pressure reaction kettle, reactor is then inserted 200 ± 5 DEG C
In baking oven, the reaction time is 24 ± 0.5h.Reaction terminates rear natural cooling and is down to room temperature, then through at filtering, washing, 60 ± 5 DEG C
12h is dried, dark gray powder is obtained, as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure ultrasound
Visible light catalyst.
Embodiment 3：
1. by 20g anhydrous hydroxides (NaOH/KOH=51.5:48.5), 0.6mmol BaCl2, 0.5mmol nano-TiOs2
It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 60% of reactor volume, and is stirred；Then sealing hydro-thermal is anti-
Kettle is answered, is put it into drying box, hydrothermal temperature is controlled at 200 DEG C, reaction time control is in 55h, and reaction is natural after terminating
Room temperature is cooled to, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, dries, and obtains BaTiO3Powder；
2. the BaTiO that 1. step obtains is weighed3Powder 100mg, and be dispersed in 100mL water, ultrasonic agitation 30min is obtained
Concentration is the BaTiO of 0.5g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=10:1 ratio, under the conditions of ultrasonic agitation to solution A in add it is corresponding anti-
Four or the six generation ammonium molybdates (ATM) that should be measured, and continue ultrasonic agitation 60min, resulting solution is labeled as B；
4. during B solution is poured into equipped with polytetrafluoroethylene (PTFE) high-temperature high-pressure reaction kettle, reactor is then inserted 200 ± 5 DEG C
In baking oven, the reaction time is 24 ± 0.5h.Reaction terminates rear natural cooling and is down to room temperature, eventually pass filter, washing, 60 ± 5 DEG C
Under dry 12h, obtain dark gray powder, i.e. Wie molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure surpass
Sound visible light catalyst.
Embodiment 4：
1. by 20g anhydrous hydroxides (NaOH/KOH=51.5:48.5), 0.6mmol BaCl2, 0.5mmol nano-TiOs2
It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 70% of reactor volume, and is stirred；Then sealing hydro-thermal is anti-
Kettle is answered, is put it into drying box, hydrothermal temperature is controlled at 200 DEG C, reaction time control is in 50h, and reaction is natural after terminating
Room temperature is cooled to, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, dries, and obtains BaTiO3Powder；
2. the BaTiO that 1. step obtains is weighed3Powder 100mg, and be dispersed in 100mL water, ultrasonic agitation 30min is obtained
Concentration is the BaTiO of 1.5g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=20:1 ratio, under the conditions of ultrasonic agitation to solution A in add it is corresponding anti-
Four or the six generation ammonium molybdates (ATM) that should be measured, and continue ultrasonic agitation 60min, resulting solution is labeled as B；
4. during B solution is poured into equipped with polytetrafluoroethylene (PTFE) high-temperature high-pressure reaction kettle, reactor is then inserted 200 ± 5 DEG C
In baking oven, the reaction time is 24 ± 0.5h.Reaction terminates rear natural cooling and is down to room temperature, eventually pass filter, washing, 60 ± 5 DEG C
Under dry 12h, obtain dark gray powder, as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure surpass
Sound visible light catalyst.
Embodiment 5：
1. by 20g anhydrous hydroxides (NaOH/KOH=51.5:48.5), 0.6mmol BaCl2, 0.5mmol nano-TiOs2
It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 80% of reactor volume, and is stirred；Then sealing hydro-thermal is anti-
Kettle is answered, is put it into drying box, hydrothermal temperature is controlled at 200 DEG C, reaction time control is in 60h, and reaction is natural after terminating
Room temperature is cooled to, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, dries, and obtains BaTiO3Powder；
2. the BaTiO that 1. step obtains is weighed3Powder 100mg, and be dispersed in 100mL water, ultrasonic agitation 30min is obtained
Concentration is the BaTiO of 2g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=100:1 ratio, under the conditions of ultrasonic agitation to solution A in add it is corresponding anti-
Four or the six generation ammonium molybdates (ATM) that should be measured, and continue ultrasonic agitation 60min, resulting solution is labeled as B；
4. during B solution is poured into equipped with polytetrafluoroethylene (PTFE) high-temperature high-pressure reaction kettle, reactor is then inserted 200 ± 5 DEG C
In baking oven, the reaction time is 24 ± 0.5h.Reaction terminates rear natural cooling and is down to room temperature, eventually pass filter, washing, 60 ± 5 DEG C
Under dry 12h, obtain dark gray powder, as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure surpass
Sound visible light catalyst.
Claims (4)
1. a kind of molybdenum bisuphide/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst, it is characterised in that：It is described to urge
Agent be with size dimension as 80nm~barium titanate (BaTiO of 120nm3) nano cubic block is in its area load thickness degree
1~10 layer of molybdenum bisuphide (MoS of 0.74~0.77nm2) be obtained；Wherein, with Ba/Mo molar ratio computings, Ba in the catalyst:
Mo=5:1~100:1.
2. molybdenum bisuphide as claimed in claim 1/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst, it is special
Levy and be：The catalyst is the barium titanate (BaTiO of ± 5nm with size dimension as 100nm3) nano cubic block is negative on its surface
Carrier layer thickness is 1~3 layer of molybdenum bisuphide (MoS of 0.74~0.77nm2) be obtained；Wherein, with Ba/Mo moles in the catalyst
Than meter, Ba:Mo=50:1~100:1.
3. the preparation side of molybdenum bisuphide described in claim 1/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst
Method, step is：
1. preparing BaTiO3Molar ratio computing, by mass ratio NaOH:KOH=51.5:48.5 anhydrous hydroxide, BaCl2,
Nano-TiO2It is added sequentially in hydrothermal reaction kettle, compactedness is controlled the 40~80% of reactor volume, and is stirred；So
After seal hydrothermal reaction kettle, in putting it into drying box, hydrothermal temperature is controlled at 200 ± 10 DEG C, the reaction time is controlled in 40h
~60h, reaction naturally cools to room temperature after terminating, products therefrom deionized water is rinsed to neutrality repeatedly, and then suction filtration, does
It is dry, that is, obtain BaTiO3Powder；
2. the BaTiO that 1. step obtains is taken3Powder is simultaneously dispersed in water, and 30 ± 5min of ultrasonic agitation, compound concentration is 0.1g//L
The BaTiO of~2g/L3Suspension, resulting solution is labeled as A；
3. Ba/Mo mol ratios Ba is pressed:Mo=5:1~100:1 ratio, under the conditions of ultrasonic agitation to solution A in add it is corresponding
Four or six generation ammonium molybdates (ATM) of reacting dose, and continue 60 ± 5min of ultrasonic agitation, resulting solution is labeled as B；
4. B solution is poured into the high-temperature high-pressure reaction kettle equipped with polytetrafluoroethylene (PTFE), reactor is then inserted into 200 ± 5 DEG C of bakings
In case, the reaction time is 24 ± 0.5h；Reaction terminates rear natural cooling and is down to room temperature, then through being done at filtering, washing, 60 ± 5 DEG C
Dry 12h, the dark gray powder for obtaining as molybdenum bisuphide/barium titanate (MoS2/BaTiO3) nano cubic block heterojunction structure ultrasound can
See photochemical catalyst.
4. molybdenum bisuphide described in claim 1 or 2/barium titanate nano cubic block heterojunction structure ultrasound visible light catalyst is in ultrasound
Application in ripple collaboration visible light catalytic cracking aquatic products hydrogen.
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| CN112044426A (en) * | 2020-10-16 | 2020-12-08 | 西安工程大学 | Barium titanate/potassium niobate composite piezoelectric photocatalyst, preparation method and application thereof |
| CN113713813A (en) * | 2021-08-31 | 2021-11-30 | 四川大学 | Ag NWs@BaTiO3Core-sheath composite piezoelectric photocatalytic material and preparation method and application thereof |
| CN115036379A (en) * | 2022-05-24 | 2022-09-09 | 杭州电子科技大学 | Molybdenum disulfide barium titanate composite nano-roll photoelectric detector and preparation method thereof |
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