CN105600824B - A kind of High-performance micro-nano multi-level structure MoS2Material, preparation method and application - Google Patents
A kind of High-performance micro-nano multi-level structure MoS2Material, preparation method and application Download PDFInfo
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- CN105600824B CN105600824B CN201610036552.7A CN201610036552A CN105600824B CN 105600824 B CN105600824 B CN 105600824B CN 201610036552 A CN201610036552 A CN 201610036552A CN 105600824 B CN105600824 B CN 105600824B
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- 238000002360 preparation method Methods 0.000 title abstract description 37
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 30
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000002077 nanosphere Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002086 nanomaterial Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- -1 polyethylene Polymers 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 238000013459 approach Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000004005 microsphere Substances 0.000 abstract 1
- 239000002736 nonionic surfactant Substances 0.000 abstract 1
- 239000010695 polyglycol Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 54
- 238000003756 stirring Methods 0.000 description 17
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 13
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 239000000314 lubricant Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 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 6
- 238000002604 ultrasonography Methods 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 230000004087 circulation Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229920006324 polyoxymethylene Polymers 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 4
- 239000000088 plastic resin Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000008118 PEG 6000 Substances 0.000 description 3
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229920002535 Polyethylene Glycol 1500 Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000001808 coupling effect Effects 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
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/1003—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- 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
- Y02E60/10—Energy storage using batteries
-
- 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 present invention relates to nano material is prepared and energy environment protection technical field, specifically a kind of High-performance micro-nano multi-level structure MoS2Material and preparation method thereof.The preparation method of the present invention makes the MoS of reaction generation by introducing a kind of non-ionic surfactant polyglycols2Ultrathin nanometer piece is self-assembled into nanosphere unit, nanosphere unit is further assembled into the microballoon with micro-nano multi-level structure, the microsphere diameter is 2～10 μm, a diameter of 50～200nm of nanosphere, a length of 100～the 300nm of the piece of nanometer sheet, a width of 100～300nm of piece, it is 2～50nm that piece is thick, nanosphere unit is intertwined to form microballoon, the 10～100m of specific surface area of microballoon2/g.This kind of MoS2Micro-nano material can not only play the advantage of nano unit high activity and efficiency, the preparation method is that a step is completed under hydrothermal conditions, have that process is simple, low energy consumption is inexpensive, short preparation period, environmentally friendly, be conducive to through engineering approaches to prepare on a large scale and apply.
Description
Technical field
A kind of the invention belongs to nano material preparation technology and application, more particularly to High-performance micro-nano multi-level structure
MoS2Raw powder's production technology.
Background technology
Two-dimentional transient metal sulfide has class graphene-structured, and its unique electronics, optical characteristics make which in lithium ion
Battery, ultracapacitor, light, electro-catalysis are produced the fields such as hydrogen, catalytic hydrogenation and are had great application prospect, and are the heat of current research
Point.Therefore, preparation research prepares and there is high performance MoS2Powder has important research justice.
Micro-nano multi-level structure is the higher-dimension for having particular geometric pattern by low-dimensional nano unit body material by assembling
Labyrinth, the class formation had both remained the high-performance of nano-particle, and the easily separated process have the advantages that large scale particle,
And contribute to guest molecule with higher specific surface area, abundant pore passage structure, its coupling effect having and cooperative effect
(gas/dyestuff/organic molecule) absorption and the transmission of material internal in material surface, be people's design construction sensitive material,
More structural model is considered when catalysis material, absorbing and storing material, energy conversion material.
The molybdenum bisuphide material of report mostly is ultrathin nanometer piece at present, or is assembled with ultrathin nanometer piece as basic structural unit
MoS2Nanosphere.And with regard to MoS2Microballoon, the preparation research that there is multilevel hierarchical structure microballoon especially not yet appear in the newspapers
Road.And develop a kind of simply effective, with low cost, environmentally friendly and can the synthetic method of synthesis application on a large scale not only can
MoS is effectively expanded2Application of the material in every field, also carries for designing and manufacturing other high performance wiener multilevel structure materials
For important evidence and technical support.
Content of the invention
It is an object of the invention to provide a kind of High-performance micro-nano multi-level structure MoS2Raw powder's production technology, and answered
Use on the fields such as absorption, air-sensitive, catalysis, lubrication.The method preparation process is simple, low cost, and yield is high, without the need for post processing,
Environmentally safe, it is easy to industrialize.
Micro-nano multi-level structure MoS of the present invention2Powder is made up of the microballoon that size is 2～10 μm, microballoon by 50～
The nanosphere unit of 200nm interweaves and constitutes, and nanosphere is formed by the ultrathin nanometer self assembly that thickness is 2～50nm.Wherein, micro-
Receive multilevel hierarchy MoS2Microballoon, the nanosphere for constituting microballoon are all even dispersion distributions.
The invention further relates to a kind of micro-nano multi-level structure MoS2Raw powder's production technology, uses the hot method of hydrothermal/solvent,
Comprise the steps of：
1) at ambient temperature, a certain amount of molybdenum salt is slowly added in solvent, is stirred to dissolving, be subsequently adding certain
The sulphur source of amount is uniformly mixing to obtain mixed solution A；
2) a certain amount of polyethylene glycol is added in the A systems for persistently stirring, obtain mixed solution B after stirring and dissolving；
3) mixed solution B is positioned in Vltrasonic device carries out ultrasonically treated, and ultrasound terminates to be transferred in reactor and carry out
Reaction；
4) black precipitate during 3) reaction terminates rear centrifugation collection step, deionized water and ethanol are alternately washed
After dry, obtain the MoS of micro-nano multi-level structure2Powder；
Described molybdenum source is 1 with the mol ratio of sulphur source:7～1:50, wherein, the molar concentration of the molybdenum source solution is 0.01
～0.5mol/L；The molar concentration of the sulphur source is 0.07mol/L～25mol/L.
The solvent is the mixed solvent of deionized water, ethylene glycol, DMF or three's composition.
The molecular weight of the polyethylene glycol is 400～6000, and polyethylene glycol is 0.05～2 with the mol ratio of molybdenum source.
The mixed solution carried out ultrasonic disperse process before reactor is added, and ultrasonic frequency is 60W～500W, surpasses
The sound time is 5min～60min.
It is another object of the present invention to by micro-nano multi-level structure MoS2Powder application is in Dye Adsorption field.
It is another object of the present invention to by micro-nano multi-level structure MoS2Powder application is in lithium ion battery negative material and electricity
Catalytic decomposition aquatic products hydrogen field.
Another object of the present invention is by micro-nano multi-level structure MoS2Powder application is in field of lubricant.
Micro-nano multi-level structure MoS prepared by the present invention2Powder, with existing MoS2Scalping structure compares beneficial effect
It is：
Micro-nano multi-level structure MoS prepared by the present invention2Powder dispersity is good, microspherulite diameter is uniform, and circularity is good, Gao Bibiao
The characteristics of area, good dispersion and easily separated recovery.Microballoon has secondary grading structure, gives its abundanter pore passage structure
And microscopic appearance, more surface-active sites can be exposed, and the absorption to dyestuff can be significantly improved for adsorbing domain
Efficiency, shortens adsorption time, has a good application prospect.
Description of the drawings
Fig. 1 is 1 micro-nano multi-level structure MoS of embodiment2The X ray diffracting spectrum of powder.
Fig. 2 is 1 micro-nano multi-level structure MoS of embodiment2The stereoscan photograph of powder.
Fig. 3 is 2 micro-nano multi-level structure MoS of embodiment2The X ray diffracting spectrum of powder.
Fig. 4 is 3 micro-nano multi-level structure MoS of embodiment2The BET test results of powder.
Specific embodiment
With reference to specific embodiment, the present invention is further elucidated with, it should be understood that these embodiments are merely to illustrate the present invention
Rather than the scope of the present invention is limited, and after the present invention has been read, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application claims limited range.
Embodiment 1
1) stir to dissolving in the deionized water that the ammonium molybdate of 1.236g is dissolved in 35ml, obtain clear solution；
2) adding the thiocarbamide of 2.284g stir in above-mentioned solution 10min to obtain mixed solution to dissolving, is subsequently adding 3g
PEG6000 stirring 1h；
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasound 30min under 100w power；
4) solution obtained in 3) is transferred in the hydrothermal reaction kettle of 50ml, 24h is heated at 180 DEG C, cold after reaction
But, gained black precipitate is centrifuged, respectively washed three times with distilled water and absolute ethyl alcohol respectively, products therefrom is passed through
50 DEG C of dryings, obtain micro-nano multi-level structure MoS2Powder.
Micro-nano multi-level structure MoS of above-mentioned preparation2The X ray diffracting spectrum of powder is as shown in figure 1, its diffraction maximum and six sides
The standard diagram of phase molybdenum bisuphide is consistent, illustrates that products therefrom is pure MoS2.The MoS of above-mentioned preparation2The ESEM of powder shines
Piece (see Fig. 2), as can be seen from the figure MoS2Microballoon of the powder for size uniform, about 5 μm of the average grain diameter of microballoon, particle
Dispersiveness, uniformity are preferable.Microballoon is interweaved by nanosphere and is constituted, and nanosphere is formed by ultrathin nanometer piece self assembly, nanosphere
Surface has abundant pleated structure.MoS2The specific surface area of microballoon is 35m2/g.
Micro-nano multi-level structure MoS of above-mentioned preparation2Powder carries out absorption property test：MoS by 5mg2Powder is added to
During 20ml concentration is for the methylene blue solution of 20mg/L, the blue degradation rate of 1min methylenes is up to 99%.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application on lithium ion battery negative shows and fills first, puts
Capacitance is 960 and 581mAh g-1, after 50 circulations, charge and discharge capacity is respectively 520 and 318mAh g-1.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application produces hydrogen field in electro-catalysis, and evolving hydrogen reaction starting is excessively electric
Position is 160mV, and when overpotential is 280mv, cathode-current density is 45mA/cm2, Tafel slope is 87mV/dec.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application in field of lubricant, by the MoS of 5wt%2It is added to heat
In plastic resin polyformaldehyde, the coefficient of friction of material is 0.13.
Embodiment 2
1) stir to dissolving in the ethylene glycol that the ammonium molybdate of 2.56g is dissolved in 35ml, obtain clear solution；
2) adding the thiocarbamide of 1.84g stir in above-mentioned solution 10min to obtain mixed solution to dissolving, is subsequently adding 1.2g
PEG6000 stirring 1h；
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasound 1h under 60w power；
4) solution obtained in 3) is transferred in the hydrothermal reaction kettle of 50ml, 24h is heated at 160 DEG C, cold after reaction
But, gained black precipitate is centrifuged, respectively washed three times with distilled water and absolute ethyl alcohol respectively, products therefrom is passed through
70 DEG C of dryings, obtain micro-nano multi-level structure MoS2Powder.
Micro-nano multi-level structure MoS of above-mentioned preparation2The X ray diffracting spectrum of powder is as shown in figure 3, its diffraction maximum and six sides
The standard diagram of phase molybdenum bisuphide is consistent, illustrates that products therefrom is pure MoS2.The MoS of above-mentioned preparation2Powder microballoon average
About 7 μm of particle diameter, the specific surface area of microballoon is 24m2/g.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder carries out absorption property test：MoS by 20mg2Powder is added
To in methylene blue solution of the 100ml concentration for 50mg/L, the blue degradation rate of 1min methylenes is up to 94%.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application on lithium ion battery negative shows and fills first, puts
Capacitance is 870 and 549mAh g-1, after 50 circulations, charge and discharge capacity is respectively 509 and 302mAh g-1.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and evolving hydrogen reaction starting overpotential is
143mV, when overpotential is 280mv, cathode-current density is 43mA/cm2, Tafel slope is 75mV/dec.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application in field of lubricant, by the MoS of 2wt%2It is added to heat
In plastic resin polyformaldehyde, the coefficient of friction of material is 0.15.
Embodiment 3
1) stir to dissolving in the DMF that the sodium molybdate of 2.5g is dissolved in 35ml, obtain clear solution；
2) adding the thiocarbamide of 5g stir in above-mentioned solution 10min to obtain mixed solution to dissolving, is subsequently adding 1.2g's
PEG1500 stirs 1h；
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasound 15min under 80w power；
4) solution obtained in 3) is transferred in the hydrothermal reaction kettle of 50ml, 18h is heated at 200 DEG C, cold after reaction
But, gained black precipitate is centrifuged, respectively washed three times with distilled water and absolute ethyl alcohol respectively, products therefrom is passed through
50 DEG C of dryings, obtain micro-nano multi-level structure MoS2Powder.
Micro-nano multi-level structure MoS of above-mentioned preparation2About 3.5 μm of the average grain diameter of powder microballoon, MoS2The BET of powder
Test result is as shown in figure 4, MoS2The specific surface area of microballoon is 46m2/g.From fig. 4, it can be seen that MoS2 micro-nano multi-level structures
Adsorption-desorption isothermal is obvious IV type thermoisopleth, and presents H3 type adsorption hysteresis rings, shows that the MoS2 for preparing is micro-
Multilevel hierarchy of receiving has that enriched to include micropore and macroporous structure.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder carries out absorption property test：MoS by 10mg2Powder is added
To in rhodamine B solution of the 20ml concentration for 20mg/L, in 3min, the degradation rate of rhodamine is up to 92%.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application on lithium ion battery negative shows and fills first, puts
Capacitance is 790 and 450mAh g-1, after 50 circulations, charge and discharge capacity is respectively 480 and 287mAh g-1.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and evolving hydrogen reaction starting overpotential is
178mV, when overpotential is 280mv, cathode-current density is 56mA/cm2, Tafel slope is 68mV/dec.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application in field of lubricant, by the MoS of 10wt%2It is added to
In thermoplastic resin polyformaldehyde, the coefficient of friction of material is 0.10.
Embodiment 4
1) ammonium molybdate of 1g is dissolved in the water of 35ml and the mixed solvent (V of ethanol compositionWater:VAlcohol=1:1) stir in
Dissolving, obtains clear solution；
2) adding the thioacetamide of 3g stir in above-mentioned solution 30min to obtain mixed solution to dissolving, is subsequently adding
The PEG1500 stirring 1h of 2g；
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasound 20min under 100w power；
4) solution obtained in 3) is transferred in the hydrothermal reaction kettle of 50ml, 18h is heated at 170 DEG C, cold after reaction
But, gained black precipitate is centrifuged, respectively washed three times with distilled water and absolute ethyl alcohol respectively, products therefrom is passed through
50 DEG C of dryings, obtain micro-nano multi-level structure MoS2Powder.
Micro-nano multi-level structure MoS of above-mentioned preparation2About 4 μm of the average grain diameter of powder microballoon, BET test results show
MoS2The specific surface area of microballoon is 57m2/g.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder carries out absorption property test：MoS by 5mg2Powder is added to
During 20ml concentration is for the rhodamine B solution of 20mg/L, in 10min, the degradation rate of rhodamine B is up to 97%.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application on lithium ion battery negative shows and fills first, puts
Capacitance is 890 and 633mAh g-1, after 50 circulations, charge and discharge capacity is respectively 580 and 356mAh g-1.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and evolving hydrogen reaction starting overpotential is
156mV, when overpotential is 280mv, cathode-current density is 67mA/cm2, Tafel slope is 57mV/dec.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application in field of lubricant, by the MoS of 8wt%2It is added to heat
In plastic resin polyformaldehyde, the coefficient of friction of material is 0.09.
Embodiment 5
1) stir to dissolving in the DMF that the sodium molybdate of 3.05g is dissolved in 35ml, obtain clear solution；
2) adding the thiocarbamide of 5.78g stir in above-mentioned solution 30min to obtain mixed solution to dissolving, is subsequently adding 0.5g
PEG6000 stirring 1h；
3) by above-mentioned 2) in the mixed solution that obtains be positioned in Vltrasonic device, ultrasound 30min under 80w power；
4) solution obtained in 3) is transferred in the hydrothermal reaction kettle of 50ml, 20h is heated at 150 DEG C, cold after reaction
But, gained black precipitate is centrifuged, respectively washed three times with distilled water and absolute ethyl alcohol respectively, products therefrom is passed through
80 DEG C of dryings, obtain micro-nano multi-level structure MoS2Powder.
Micro-nano multi-level structure MoS of above-mentioned preparation2About 4 μm of the average grain diameter of powder, BET test results show MoS2Micro-
The specific surface area of ball is 35m2/g.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder carries out absorption property test：MoS by 10mg2Powder is added
To in rhodamine B solution of the 50ml concentration for 10mg/L, in 5min, the degradation rate of rhodamine B is up to 92%.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application on lithium ion battery negative shows and fills first, puts
Capacitance is 920mAh g-1With 643mAh g-1, after 50 circulations, charge and discharge capacity is respectively 640 and 567mAh g-1.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application produces hydrogen in electro-catalysis, and evolving hydrogen reaction starting overpotential is
180mV, when overpotential is 280mv, cathode-current density is 57mA/cm2, Tafel slope is 69mV/dec.
Micro-nano multi-level structure MoS by above-mentioned preparation2Powder application in field of lubricant, by the MoS of 5wt%2It is added to heat
In plastic resin polyformaldehyde, the coefficient of friction of material is 0.11.
Claims (4)
1. a kind of High-performance micro-nano multi-level structure MoS2Material, it is characterised in that：MoS2There is a diameter of 2～10 μm of microspheroidal
Looks, the microballoon are to be interweaved to form by the nanosphere unit of a large amount of size uniformities, and microballoon specific surface area is 10～100m2/ g,
A diameter of 50～200nm of the nanosphere unit of composition microballoon, nanosphere is from group by the ultrathin nanometer piece that thickness is 2～50nm
Dress is formed, and molybdenum source and sulphur source are dissolved in deionized water, ethylene glycol, the mixing of DMF or three's any combination specifically
In solvent, then in the solution, a certain amount of surfactant polyethylene is added, stirred to after being completely dissolved, will be mixed molten
Liquid is transferred in hydrothermal device, carries out the sediment that hydro-thermal reaction obtains black, by sediment with 1000r/min～10000r/
Alternately washed using distilled water and absolute ethyl alcohol after min rotating speed centrifugations successively, vacuum at 30 DEG C～100 DEG C again
3h～30h is dried, MoS is obtained2Micro-nano material, the molybdenum source are 1 with the mol ratio of sulphur source:7～1:50, wherein, the molybdenum source
The molar concentration of solution is 0.01～0.5 mol/L；The molar concentration of the sulphur source solution is 0.07mol/L～25mol/L.
2. according to High-performance micro-nano multi-level structure MoS described in claim 12, it is characterised in that:The molecule of the polyethylene glycol
Measure as 400～6000, the polyethylene glycol is 0.05～2 with the mol ratio of molybdenum source.
3. High-performance micro-nano multi-level structure MoS according to claim 12, it is characterised in that the mixed solution is being added instead
Ultrasonic disperse process is carried out before answering kettle, and ultrasonic power is 60W～500W, and ultrasonic time is 5min～60min.
4. High-performance micro-nano multi-level structure MoS according to claim 12, it is characterised in that the compactedness of hydrothermal reaction kettle
For 25 %～45 %；The hydrothermal temperature be 100 °C～240 DEG C, the hydro-thermal reaction time be 1h～
60 h.
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| CN107199040B (en) * | 2017-07-06 | 2020-07-31 | 中国科学院福建物质结构研究所 | Molybdate nano array and preparation method and application thereof |
| CN108314084B (en) * | 2018-02-09 | 2019-12-20 | 西北工业大学 | Preparation method of metal phase molybdenum disulfide nanospheres |
| CN108383169A (en) * | 2018-04-04 | 2018-08-10 | 三峡大学 | A kind of preparation method and applications of ternary layered Transition-metal dichalcogenide |
| CN108607581B (en) * | 2018-05-11 | 2020-11-24 | 湖北民族学院 | Synthetic method and application of molybdenum disulfide material with adsorption-photocatalytic performance |
| CN108587736A (en) * | 2018-05-30 | 2018-09-28 | 郭迎庆 | A kind of preparation method of inorganic modified plant base lube oil additive |
| CN109360987A (en) * | 2018-10-29 | 2019-02-19 | 江苏师范大学 | A kind of preparation method of high-tap density anode material of lithium-ion battery |
| CN109650450B (en) * | 2019-01-18 | 2021-03-09 | 三峡大学 | Hollow MoS2Preparation method and application of microspheres |
| CN109908921B (en) * | 2019-03-11 | 2022-02-01 | 三峡大学 | MoS2NiO blankCore microsphere material, preparation method and application |
| CN110526294B (en) * | 2019-09-24 | 2022-03-08 | 暨南大学 | Synthetic method and application of sintering-resistant molybdenum disulfide |
| CN112028121B (en) * | 2020-09-28 | 2021-08-03 | 四川大学 | Preparation method of amorphous molybdenum disulfide nano material based on photocatalytic synthesis |
| CN114318397A (en) * | 2021-12-07 | 2022-04-12 | 南京信息工程大学 | Molybdenum-based electrocatalyst, preparation method thereof, bifunctional electrolytic cell and application thereof |
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