CN106807407A - A kind of nanometer nuclear shell spherical molybdenum trioxide/molybdenum bisuphide and preparation method thereof - Google Patents
A kind of nanometer nuclear shell spherical molybdenum trioxide/molybdenum bisuphide and preparation method thereof Download PDFInfo
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- CN106807407A CN106807407A CN201611175666.6A CN201611175666A CN106807407A CN 106807407 A CN106807407 A CN 106807407A CN 201611175666 A CN201611175666 A CN 201611175666A CN 106807407 A CN106807407 A CN 106807407A
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 113
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000011733 molybdenum Substances 0.000 title claims abstract description 47
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 90
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 71
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000005864 Sulphur Substances 0.000 claims abstract description 45
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 31
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 24
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 16
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 53
- 238000013019 agitation Methods 0.000 description 27
- 239000007864 aqueous solution Substances 0.000 description 22
- 239000011258 core-shell material Substances 0.000 description 20
- 239000000047 product Substances 0.000 description 20
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 16
- 239000011609 ammonium molybdate Substances 0.000 description 16
- 235000018660 ammonium molybdate Nutrition 0.000 description 16
- 229940010552 ammonium molybdate Drugs 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 14
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 9
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000000975 dye Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910015667 MoO4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 235000007686 potassium Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—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
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method, comprises the following steps：Molybdenum source, deionized water and cationic surfactant are mixed, molybdenum source solution is obtained；Sulphur source and deionized water are mixed, sulphur source solution is obtained；Molybdenum source solution and sulphur source solution are mixed, mixed liquor is obtained, and adjusts the pH of the mixed liquor to alkalescence；Hydro-thermal reaction is carried out to the mixed liquor after regulation pH, product is obtained；The product is washed and dried successively, the nanometer nuclear shell spherical MoO is obtained3/MoS2.Obtained nanometer nuclear shell spherical MoO3/MoS2With excellent photocatalysis effect, a small amount of nanometer nuclear shell spherical MoO is being added3/MoS2, in the short period of time can complete photocatalytically degradating organic dye.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of nanometer nuclear shell spherical MoO3/MoS2And its preparation side
Method.
Background technology
Nano molybdenum disulfide (MoS2) because with high-specific surface area and good light, electricity, lubrication, catalytic performance, making it
It is with a wide range of applications at aspects such as electron probe, oil catalysis, hydrogen storage material, friction, lubrication and solar cells.
Molybdenum bisuphide is direct narrow gap semiconductor, and energy gap is 1.29-1.9eV, close to the optimal taboo of solar cell material
Bandwidth (1.45eV).Therefore, it also has wide application in photocatalysis field.
Performance and its preparation method, pattern, size because of inorganic nano material etc. have a close relationship, therefore scientific research people
Member continuously attempts to various methods to prepare the nano molybdenum disulfide of different-shape, size, to improve its corresponding performance.
The current existing many kinds of its preparation method, such as chemical vapour deposition technique, high temperature vulcanized method, electrochemical process, hydro-thermal and solvent heat
Method, high temperature pyrolytic cracking (HTP), Physical, microemulsion method and natural minerals method of purification etc., by above-mentioned various methods, can be obtained difference
The nano molybdenum disulfide of pattern and size, such as nano wire, nanobelt, nanotube, nanometer rods, Nano microsphere and individual layer sheet
Deng.But, its corresponding performance still has much room for improvement.
In order to further improve its performance, the A of Chinese patent literature CN 105148947 disclose a kind of TiO2/MoS2It is compound
The preparation method and photocatalytic applications of material.The method includes：Hydrolysis titanium source prepares pattern rule, the TiO of size uniformity2It is micro-
Scale particles, add molybdenum source, sulphur source, and TiO is prepared by hydro-thermal method2/MoS2Core-shell particles.The core-shell particles are in visible ray
Under the conditions of, there is certain light degradation effect to organic dyestuff.
But, TiO obtained in above-mentioned technology2/MoS2Core-shell particles are still deposited during photocatalytically degradating organic dye
Defect the photocatalytic degradation time is long, more than photochemical catalyst addition, therefore, how to provide a kind of photocatalytic degradation time it is short,
The few photochemical catalyst of photochemical catalyst addition is a technical problem of this area urgent need to resolve.
The content of the invention
Therefore, to be solved by this invention is that existing photochemical catalyst has that the photocatalytic degradation time is long, photochemical catalyst addition
The many defects of amount, so provide that a kind of photocatalytic degradation time is short, photochemical catalyst addition less and the good nuclear shell ball of photocatalysis effect
Shape MoO3/MoS2And preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
Nanometer nuclear shell spherical MoO provided by the present invention3/MoS2Preparation method, comprise the following steps：
Molybdenum source, deionized water and cationic surfactant are mixed, molybdenum source solution is obtained；Sulphur source and deionized water are mixed
Close, sulphur source solution is obtained；
Molybdenum source solution and sulphur source solution are mixed, mixed liquor is obtained, and adjusts the pH of the mixed liquor to alkalescence；
Hydro-thermal reaction is carried out to the mixed liquor after regulation pH, product is obtained；
The product is washed and dried successively, the nanometer nuclear shell spherical MoO is obtained3/MoS2。
Preferably, the mol ratio of the molybdenum source, the sulphur source and cetyl trimethylammonium bromide is (1-2)：(1-3)：
(0.1-0.4)；
The concentration in the molybdenum source Molybdenum in Solution source is 0.1-0.5mmol/ml；
The concentration of sulphur source is 0.3-0.5mmol/ml in the sulphur source solution.
Preferably, the volume ratio of the molybdenum source solution and the sulphur source solution is 1：(1-2)；
The pH is 8-12.
Further, the mixed liquor is to drop to the molybdenum source solution by 0.005-0.05ml/s by the sulphur source solution
In.
Preferably, the temperature of the hydro-thermal reaction is 170 DEG C~200 DEG C, and the time is 12h-24h.
Preferably, the dry temperature is 60-70 DEG C, and the time is 6-8h.
Further, the washing is to be washed with deionized water and ethanol successively；
The hydro-thermal reaction is carried out in autoclave.
Further, the molybdenum source is at least one in molybdenum trioxide, ammonium molybdate, sodium molybdate and potassium molybdate；
The sulphur source be potassium rhodanide, sodium sulfocyanate, thiocarbamide, sodium thiosulfate, potassium thiosulfate and sulphur powder at least
It is a kind of；
The cationic surfactant is cetyl trimethylammonium bromide.
Present invention also offers the nanometer nuclear shell spherical MoO as obtained in above-mentioned preparation method3/MoS2。
Further, the nanometer nuclear shell spherical MoO3/MoS2A diameter of 1~2 μm；
The nanometer nuclear shell spherical MoO3/MoS2Shell MoS2Thickness be 100-150nm, its surface irregularity, and distribution
Hole.
Compared with prior art, the present invention has the advantages that：
(1) the nanometer nuclear shell spherical MoO that the embodiment of the present invention is provided3/MoS2Preparation method, first by molybdenum source, deionized water and
Cationic surfactant mixes, and molybdenum source solution is obtained；Sulphur source and deionized water are mixed, sulphur source solution is obtained；Then by molybdenum
Source solution and sulphur source solution mix, and obtain mixed liquor, and adjust the pH of the mixed liquor to alkalescence；Again to the mixing after regulation pH
Liquid carries out hydro-thermal reaction, obtains product；Finally product is washed successively and is dried, obtained nanometer nuclear shell spherical
MoO3/MoS2.In above-mentioned preparation method, cationic surfactant cationic can form many vesicas in deionized water, this
A little vesicas meeting wrapping portion molybdenum sources, another part molybdenum source forms MoO in deionized water4 2-Ion is absorbed by electrostatic interaction
To the outer surface layer of vesica, the S discharged from sulphur source-Hydro-thermal reaction can occur therewith, then through dried process after, finally give with
MoO3For core, with MoS2It is the nanometer nuclear shell spherical MoO of shell3/MoS2, nanometer nuclear shell spherical MoO3/MoS2With excellent photocatalysis effect,
Adding a small amount of nanometer nuclear shell spherical MoO3/MoS2, in the short period of time can complete photocatalytically degradating organic dye.
(2) the nanometer nuclear shell spherical MoO that the embodiment of the present invention is provided3/MoS2Preparation method, by the pH for controlling mixed liquor
In 8-12, there is provided an alkaline environment, be conducive to nanometer nuclear shell spherical MoO3/MoS2The formation of center, there is provided nucleation rate；Furthermore, will
Sulphur source solution is dropped in molybdenum source solution by 0.005-0.05ml/s, the S that can be allowed in sulphur source solution-In molybdenum source solution
MoO4 2-Fully reaction, is difficult to reunite, and then forms the homogeneous core shell structure of pattern, further increasing nucleation rate, final logical
Cross aforesaid operations and improve nanometer nuclear shell spherical MoO in unit mass photochemical catalyst3/MoS2Accounting, finally improve photocatalysis effect
Really, the addition of photocatalysis time and photochemical catalyst is reduced.
(3) the nanometer nuclear shell spherical MoO that the embodiment of the present invention is provided3/MoS2Preparation method, wherein the phase between each parameter
Mutually coordinate and be beneficial to obtain nanometer nuclear shell spherical MoO as much as possible with effect, effect on the whole3/MoS2；Furthermore in the process of nucleation
In, wrapped core can be decomposed and discharge gas, caused and formed on shell many holes and rough surface, these structures
Formation be conducive to improving nanometer nuclear shell spherical MoO3/MoS2Specific surface area, finally improve its photocatalysis effect.
(4) the nanometer nuclear shell spherical MoO that the embodiment of the present invention is provided3/MoS2Preparation method, with low production cost, be easy to
Batch production, the uniform advantage of product particle size.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the MoO of core shell structure in the embodiment of the present invention 13/MoS2SEM figure.
Fig. 2 is the MoO of core shell structure in the embodiment of the present invention 13/MoS2XRD.
Fig. 3 is the MoO of core shell structure in the embodiment of the present invention 13/MoS2TEM figure.
Specific embodiment
In order to the object, technical solutions and advantages of the present invention are better described, below in conjunction with specific embodiment to this hair
It is bright to be described further.The present invention can be embodied in many different forms, and should not be construed as limited to set forth herein
Embodiment.Conversely, there is provided these embodiments so that the disclosure will be thorough and complete, and will it is of the invention design fill
Divide and convey to those skilled in the art, the present invention will only be defined by the appended claims.
Photocatalysis experiment instrument is the life of Beijing Zhong Jiaojin sources Science and Technology Ltd. in following each embodiments and comparative example
The CEL-LAX types simulated visible light reaction instrument (light source is 500W xenon lamps) of product.
The photocatalysis process of the test of sample is as follows described in following each embodiments and comparative example：
1) aqueous solution of methylene blue of 60mg/L is prepared；Prepare the rhodamine B aqueous solution of 60mg/L；
2) the above-mentioned each aqueous solution of 60ml is taken to be added separately in quartz ampoule；
3) again to the photochemical catalyst that 5mg is separately added into above-mentioned each quartz ampoule, and it is well mixed after, be transferred to simulated visible light
In reaction instrument, after standing 60min in dark, xenon lamp is opened, light-catalyzed reaction is carried out under continuous magnetic agitation；
4) respectively in 0min, 20min, 30min, 40min, 50min, 60min, the above-mentioned dye solutions of 4ml are taken and is put into 5ml
Centrifuge tube in be centrifuged, and take supernatant, pour into cuvette, UV-Vis spectrometer measures its absorbance, obtains light drop
Solution rate.
Embodiment 1
Present embodiments provide a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method includes following step
Suddenly：
(1) 0.4319g molybdenum trioxides (MoO is weighed3) (3mmol) is added in the deionized water of 20ml, under magnetic agitation,
Molybdenum trioxide suspension is obtained, and is added thereto to 0.07287g (0.2mmol) cetyl trimethylammonium bromide (CTAB), magnetic
Power stirring makes it be completely dissolved in molybdenum trioxide suspension, and molybdenum source solution is obtained；
0.8017g potassium rhodanides (KSCN) (8mmol) are weighed to be added in the deionized water of 20ml, under magnetic agitation, system
Obtain sulphur source solution；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.02ml/s, magnetic agitation makes both mix
It is even, and its pH is adjusted to 8, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 170 DEG C, time are 24h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 6h is dried at 70 DEG C, nanometer nuclear shell spherical MoO is obtained3/MoS2；
To above-mentioned nanometer nuclear shell spherical MoO3/MoS2Tested, corresponding test result is as follows：
Fig. 1 is the MoO of core shell structure3/MoS2SEM figure, can be learnt from Fig. 1：It it is 1.5 μm which form average diameter
MoO3Core, average thickness are the MoS of 150nm2Shell, its surface irregularity, and it is dispersed with hole.
Fig. 2 is the MoO of core shell structure3/MoS2XRD, can be learnt from Fig. 2：* it is MoO3(020) characteristic peak, show
There is MoO3Core, other characteristic peaks and pure MoS2Peak matches, and shows there is MoS2Generation, it was demonstrated that MoO3/MoS2Core shell structure
Formed.
Fig. 3 is the MoO of core shell structure3/MoS2TEM figure, can be learnt from Fig. 3：The MoO of core shell structure3/MoS2Center
For spherical, the outer surface of ball is attached with flaky texture.
Photocatalysis experiment shows：Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, aqueous solution of methylene blue is dropped completely
Solution；Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, the degradation rate of its rhodamine B aqueous solution to 60mg/L reaches 99.8%
Embodiment 2
Present embodiments provide a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method includes following step
Suddenly：
(1) ammonium molybdate for weighing 2mmol is added in the deionized water of 20ml, under magnetic agitation, obtains ammonium molybdate water-soluble
Liquid, and the cetyl trimethylammonium bromide (CTAB) of 0.2mmol is added thereto to, magnetic agitation makes it be completely dissolved in ammonium molybdate
In the aqueous solution, molybdenum source solution is obtained；
Weigh 6mmol thiocarbamides to be added in the deionized water of 20ml, under magnetic agitation, sulphur source solution is obtained；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.05ml/s, magnetic agitation makes both mix
It is even, and its pH is adjusted to 9, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 200 DEG C, time are 12h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 8h is dried at 60 DEG C, nanometer nuclear shell spherical MoO is obtained3/MoS2；
To above-mentioned nanometer nuclear shell spherical MoO3/MoS2Tested, corresponding test result is as follows：
SEM tests show：Which form the MoO that average diameter is 1 μm3Core, average thickness are the MoS of 100nm2Shell, its table
Face is uneven, and is dispersed with hole.
XRD shows：It is MoO3/MoS2Core shell structure.
TEM charts are bright：The MoO of core shell structure3/MoS2Center for spherical, the outer surface of ball is attached with flaky texture.
Photocatalysis experiment shows：Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, aqueous solution of methylene blue is dropped completely
Solution；Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, the degradation rate of its rhodamine B aqueous solution to 60mg/L reaches 99.6%.
Embodiment 3
Present embodiments provide a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method includes following step
Suddenly：
(1) ammonium molybdate for weighing 4mmol is added in the deionized water of 20ml, under magnetic agitation, obtains ammonium molybdate water-soluble
Liquid, and the cetyl trimethylammonium bromide (CTAB) of 0.8mmol is added thereto to, magnetic agitation makes it be completely dissolved in ammonium molybdate
In the aqueous solution, molybdenum source solution is obtained；
Weigh 2mmol sodium thiosulfate to be added in the deionized water of 20ml, under magnetic agitation, sulphur source solution is obtained；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.008ml/s, magnetic agitation makes both mix
It is even, and its pH is adjusted to 12, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 180 DEG C, time are 20h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 7h is dried at 65 DEG C, nanometer nuclear shell spherical MoO is obtained3/MoS2；
To above-mentioned nanometer nuclear shell spherical MoO3/MoS2Tested, corresponding test result is as follows：
SEM tests show：Which form the MoO that average diameter is 1.4 μm3Core, average thickness are the MoS of 130nm2Shell, its
Surface irregularity, and it is dispersed with hole.
XRD shows：It is MoO3/MoS2Core shell structure.
TEM charts are bright：The MoO of core shell structure3/MoS2Center for spherical, the outer surface of ball is attached with flaky texture.
Photocatalysis experiment shows：Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, aqueous solution of methylene blue is dropped completely
Solution；Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, the degradation rate of its rhodamine B aqueous solution to 60mg/L reaches 99.7%.
Embodiment 4
Present embodiments provide a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method includes following step
Suddenly：
(1) ammonium molybdate for weighing 3mmol is added in the deionized water of 20ml, under magnetic agitation, obtains ammonium molybdate water-soluble
Liquid, and the cetyl trimethylammonium bromide (CTAB) of 0.4mmol is added thereto to, magnetic agitation makes it be completely dissolved in ammonium molybdate
In the aqueous solution, molybdenum source solution is obtained；
Weigh 5mmol sulphur powders to be added in the deionized water of 20ml, under magnetic agitation, sulphur source solution is obtained；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.005ml/s, magnetic agitation makes both mix
It is even, and its pH is adjusted to 11, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 190 DEG C, time are 18h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 6.5h is dried at 68 DEG C, nanometer nuclear shell spherical MoO is obtained3/MoS2；
To above-mentioned nanometer nuclear shell spherical MoO3/MoS2Tested, corresponding test result is as follows：
SEM tests show：Which form the MoO that average diameter is 1.3 μm3Core, average thickness are the MoS of 140nm2Shell, its
Surface irregularity, and it is dispersed with hole.
XRD shows：It is MoO3/MoS2Core shell structure.
TEM charts are bright：The MoO of core shell structure3/MoS2Center for spherical, the outer surface of ball is attached with flaky texture.
Photocatalysis experiment shows：Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, aqueous solution of methylene blue is dropped completely
Solution；Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, the degradation rate of its rhodamine B aqueous solution to 60mg/L reaches 99.7%.
Embodiment 5
Present embodiments provide a kind of nanometer nuclear shell spherical MoO3/MoS2And preparation method thereof.The preparation method includes following step
Suddenly：
(1) ammonium molybdate for weighing 3mmol is added in the deionized water of 20ml, under magnetic agitation, obtains ammonium molybdate water-soluble
Liquid, and the cetyl trimethylammonium bromide (CTAB) of 0.3mmol is added thereto to, magnetic agitation makes it be completely dissolved in ammonium molybdate
In the aqueous solution, molybdenum source solution is obtained；
Weigh 5mmol potassium thiosulfates to be added in the deionized water of 20ml, under magnetic agitation, sulphur source solution is obtained；
(2) the sulphur source solution and the molybdenum source solution are mixed, magnetic agitation is well mixed both, and adjusts its pH
To 9, mixed liquor is obtained；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 180 DEG C, time are 21h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 7h is dried at 70 DEG C, nanometer nuclear shell spherical MoO is obtained3/MoS2；
To above-mentioned nanometer nuclear shell spherical MoO3/MoS2Tested, corresponding test result is as follows：
SEM tests show：Which form the MoO that average diameter is 1.5 μm3Core, average thickness are the MoS of 110nm2Shell.
XRD shows：It is MoO3/MoS2Core shell structure.
TEM charts are bright：The MoO of core shell structure3/MoS2Center for spherical, the outer surface of ball is attached with flaky texture.
Photocatalysis experiment shows：Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, to the degradation rate of aqueous solution of methylene blue
Reach 99.9%；Above-mentioned nanometer nuclear shell spherical MoO3/MoS2After 60min, the degradation rate of its rhodamine B aqueous solution to 60mg/L reaches
To 99.0%.
Comparative example 1
This comparative example provides a kind of MoO3/MoS2And preparation method thereof.The preparation method comprises the following steps：
(1) 0.4319g molybdenum trioxides (MoO is weighed3) (3mmol) is added in the deionized water of 20ml, under magnetic agitation,
Molybdenum trioxide suspension is obtained, and is added thereto to 0.07287g (0.2mmol) cetyl trimethylammonium bromide (CTAB), magnetic
Power stirring makes it be completely dissolved in molybdenum trioxide suspension, and molybdenum source solution is obtained；
0.8017g potassium rhodanides (KSCN) (8mmol) are weighed to be added in the deionized water of 20ml, under magnetic agitation, system
Obtain sulphur source solution；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.02ml/s, magnetic agitation makes both mix
It is even, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 170 DEG C, time are 24h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 6h is dried at 70 DEG C, MoO is obtained3/MoS2；
To above-mentioned MoO3/MoS2Photocatalysis experimental test is carried out, corresponding test result is as follows：Above-mentioned MoO3/MoS2
After 60min, the degradation rate to aqueous solution of methylene blue is 80%, and the degradation rate to the rhodamine B aqueous solution is 65%.
Comparative example 2
This comparative example provides a kind of MoO3/MoS2And preparation method thereof.The preparation method comprises the following steps：
(1) ammonium molybdate for weighing 4mmol is added in the deionized water of 20ml, under magnetic agitation, obtains ammonium molybdate water-soluble
Liquid, and the neopelex of 0.8mmol is added thereto to, magnetic agitation makes it be completely dissolved in ammonium molybdate aqueous solution,
Molybdenum source solution is obtained；
Weigh 2mmol sodium thiosulfate to be added in the deionized water of 20ml, under magnetic agitation, sulphur source solution is obtained；
(2) in the sulphur source solution being dropped into the molybdenum source solution by 0.008ml/s, magnetic agitation makes both mix
It is even, and its pH is adjusted to 12, obtain mixed liquor；
(3) hydro-thermal reaction is carried out in the autoclave that the mixed liquor is moved to 50ml, and controls the temperature of hydro-thermal reaction
Spend for 180 DEG C, time are 20h, obtain product；
(4) product is taken out from autoclave, and naturally cools to room temperature, then use deionized water successively
With ethanol washing, centrifugation, then at being placed in vacuum drying chamber, and in 7h is dried at 65 DEG C, MoO is obtained3/MoS2；
To above-mentioned MoO3/MoS2Photocatalysis experimental test is carried out, corresponding test result is as follows：Above-mentioned MoO3/MoS2
After 60min, the degradation rate to aqueous solution of methylene blue is 63%, and the degradation rate to the rhodamine B aqueous solution is 45%.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of nanometer nuclear shell spherical MoO3/MoS2Preparation method, comprise the following steps：
Molybdenum source, deionized water and cationic surfactant are mixed, molybdenum source solution is obtained；Sulphur source and deionized water are mixed,
Sulphur source solution is obtained；
Molybdenum source solution and sulphur source solution are mixed, mixed liquor is obtained, and adjusts the pH of the mixed liquor to alkalescence；
Hydro-thermal reaction is carried out to the mixed liquor after regulation pH, product is obtained；
The product is washed and dried successively, the nanometer nuclear shell spherical MoO is obtained3/MoS2。
2. preparation method according to claim 1, it is characterised in that the molybdenum source, the sulphur source and cetyl front three
The mol ratio of base ammonium bromide is (1-2)：(1-3)：(0.1-0.4)；
The concentration in the molybdenum source Molybdenum in Solution source is 0.1-0.5mmol/ml；
The concentration of sulphur source is 0.3-0.5mmol/ml in the sulphur source solution.
3. preparation method according to claim 1 and 2, it is characterised in that the molybdenum source solution and the sulphur source solution
Volume ratio is 1：(1-2)；
The pH is 8-12.
4. the preparation method according to any one of claim 1-3, it is characterised in that the mixed liquor is by the sulphur source
Solution is dropped in the molybdenum source solution by 0.005-0.05ml/s.
5. the preparation method according to any one of claim 1-4, it is characterised in that the temperature of the hydro-thermal reaction is
170 DEG C~200 DEG C, the time is 12h-24h.
6. the preparation method according to any one of claim 1-5, it is characterised in that the dry temperature is 60-70
DEG C, the time is 6-8h.
7. the preparation method according to any one of claim 1-6, it is characterised in that the washing to use deionization successively
Water and ethanol are washed；
The hydro-thermal reaction is carried out in autoclave.
8. the preparation method according to any one of claim 1-7, it is characterised in that the molybdenum source is molybdenum trioxide, molybdenum
At least one in sour ammonium, sodium molybdate and potassium molybdate；
The sulphur source is at least one in potassium rhodanide, sodium sulfocyanate, thiocarbamide, sodium thiosulfate, potassium thiosulfate and sulphur powder；
The cationic surfactant is cetyl trimethylammonium bromide.
9. nanometer nuclear shell spherical MoO obtained in the preparation method any one of claim 1-83/MoS2。
10. nanometer nuclear shell spherical MoO according to claim 93/MoS2, it is characterised in that the nanometer nuclear shell spherical MoO3/MoS2's
A diameter of 1~2 μm；
The nanometer nuclear shell spherical MoO3/MoS2Shell MoS2Thickness be 100-150nm, its surface irregularity, and be dispersed with hole
Hole.
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