CN108128805A - A kind of preparation method of molybdenum disulfide hollow ball - Google Patents
A kind of preparation method of molybdenum disulfide hollow ball Download PDFInfo
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- CN108128805A CN108128805A CN201611087573.8A CN201611087573A CN108128805A CN 108128805 A CN108128805 A CN 108128805A CN 201611087573 A CN201611087573 A CN 201611087573A CN 108128805 A CN108128805 A CN 108128805A
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- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The present invention relates to a kind of preparation methods of the flower-shaped hollow ball of molybdenum disulfide.The present invention includes the following steps：A certain proportion of mixed solution is configured and makees solvent, surfactant is dissolved in above-mentioned solvent；Sulphur source, molybdenum source, reducing agent is added in be uniformly mixed；The mixed solution is moved into autoclave, constant temperature is kept for certain time；Be cooled to room temperature, detach, wash, be dried after the flower-shaped hollow ball of molybdenum disulfide.The flower-shaped hollow ball spherical structure of molybdenum disulfide prepared by the present invention is regular, and flower-shaped lamella arrangements are loose, grain size and wall thickness is uniform adjustable and structural stability is good.The building-up process is simple, of low cost, synthesizer is simple, modulating method is simple, operable row is strong, product purity is high, and yield is high.The preparation method of the present invention is expected to be used for the adjustable transient metal sulfide of synthesis appearance structure and transition metal oxide.
Description
Technical field
The present invention relates to the preparation methods of the flower-shaped hollow ball of molybdenum disulfide, belong to micro Nano material preparation field.
Background technology
Molybdenum disulfide has the layer structure of hexagonal crystal system, is combined between layers by weaker Van der Waals force, layer
It is inside that active force is combined by stronger covalent bond.Due to its heterogeneous layered structure feature, it is widely used in solid
In the fields such as lubricant, hydrogenation catalyst, intercalation material.As molybdenum disulfide application field is constantly expanded, people are to two sulphur
Change the grain size of molybdenum and pattern proposes that higher requires, therefore new preparation method developed be used to prepare tool successively in more detail
There is the micro/nano level molybdenum disulfide of special construction and pattern.In recent years, researchers employ gas chemistry synthetic method in succession, preceding
Drive body decomposition method, the methods of hydro-thermal method, hydrothermal method, masterplate method be prepared for spherical shape, threadiness, tubulose, flower-shaped molybdenum disulfide it is micro-/receive
Rice grain is that have different-shape and the micro-/ nano particle of structure by what molybdenum disulfide nano sheet was self-assembly of.But it closes at present
It is fewer in the relevant report of hollow-core construction molybdenum disulfide material preparation method.
[CN105140518A] discloses a kind of nanocage hollow fullerene-like molybdenum disulfide and preparation method thereof and should
With.This method is by (the NH of 1mol4)2MoS4It is dissolved in the N-Methyl pyrrolidone solvent of 10L, after 3-5 hours ultrasonic, hydrazine hydrate
Make reducing agent, be heated to 80 DEG C be stirred at reflux reaction 12 hours after, cool down, centrifuge, separation, the product being dried to obtain is at 800 DEG C
Inert atmosphere in be heat-treated after, obtain nanocage hollow fullerene-like molybdenum disulfide.But this method wants consersion unit
Ask higher, reaction time is longer.Lina Ye etc. are reported in Chem.Mater.2007,19,6331-6337 uses MoO3,
Bu4The reagents such as NBr, NaF, NaSCN are prepared for by two for 6 hours after the reaction 8 hours of 160 DEG C of high pressure hydro-thermal, then in 220 DEG C of reactions
The hollow cage-shape structure that the accumulation of molybdenum sulfide nanometer sheet forms.Yinghua Tan et al. are in Journal of materials
Chemistry C, 2014,2,5422 report and use Na2MoO4H2O、(C2H5) NS and H2C2O4Presoma hydro-thermal method is done 200
Product is obtained after reacting 22h under the conditions of DEG C, which is mainly made of the hollow ball of the molybdenum disulfide of two kinds of different-grain diameters, grain
Diameter is respectively distributed to 1 μm and 200nm or so.[CN102701281B] discloses a kind of preparation side of flower-shaped molybdenum disulfide hollow ball
Method.This method is by (NH4)2MoO4、CS(NH2)2And NH2After mixing, the pH value of solution is adjusted for OHHCl and surfactant
After 5-6.5, solution is moved into reaction kettle, isothermal reaction is cooled to room temperature, and is repeatedly filtered, and washing is dried to obtain a diameter of
1-2 microns of flower-shaped hollow ball.
Although molybdenum disulfide hollow-core construction made from Yi Shang several method, size distribution ranges are wider, sphericity is low,
Wall thickness is larger, easily reunites, appearance and size is difficult to control, and technological process is relative complex, and productivity ratio is compared with low production cost relatively
It is high.
Invention content：
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of size (grain size, wall thickness) it is uniform, can
Control the preparation method of molybdenum disulfide hollow ball.The molybdenum disulfide hollow ball is assembled by molybdenum disulfide nano sheet, grain size
In 1.2-2.5 μm, wall thickness 120-200nm.
Process of the present invention is using the mild solvent structure of a step, the preparation method of the flower-shaped hollow ball of molybdenum disulfide
Include the following steps：
1st, (1) configuration different volumes than the mixed solution of second alcohol and water make solvent, by surfactant be dissolved in ethyl alcohol and
In water mixed solution, after stirring evenly, with molybdenum source, sulphur source is added with stirring after mixing, N is added in2H4+H2O；
(2) it after the solution prepared in (1) is stirred evenly, moves into reaction kettle, sealing is heated to certain temperature, constant temperature
It after a period of time, is cooled to room temperature, obtains product；
(3) above-mentioned product is detached, vacuum drying obtains the flower-shaped hollow ball of molybdenum disulfide.
2nd, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, wherein the solvent is nothing
The volume ratio of the mixed solution of water-ethanol and water, absolute ethyl alcohol and water is 0.01-0.6, is preferably 0.025-0.45.
3rd, the preparation method of the controllable molybdenum disulfide hollow ball of size of the present invention, wherein the surfactant is
CTAB (cetyl trimethylammonium bromide), PEG (polyethylene glycol), PVP (polyvinylpyrrolidone) or SDBS.It was prepared at this
Cheng Zhong, surfactant molecule self-service dress in mixed solution form positively charged spherical micelle, and hydrophobic alkyl is round and round
Gather in the inside of sphere, hydrophilic functional groups are distributed in the surface of sphere.The effect of the micella lifting plate agent.This experimentation passes through
The volume ratio of each component in mixed solution is adjusted, changes the critical micelle concentration that surfactant forms micella, generates glue
Gibb ' s free energys, aggregation number of micelle and the micella Size Distribution of beam.It is acted on by attractive coulombic force, negatively charged molybdate is easily inhaled
The surface of micella is attached to, generation H is hydrolyzed with thiocarbamide2Reduction reaction generation molybdenum disulfide occurs for S.Surfactant molecule not only hinders
Hinder the growth of molybdenum disulfide nano sheet and change the accumulation mode of molybdenum disulfide nano sheet, and then change flower-like nanometer two
The size and wall thickness of molybdenum sulfide hollow ball finally obtain flower-shaped hollow molybdenum disulfide microspheres, and the molar concentration of surfactant is 3-
10mmol/L。
4th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention；Wherein described molybdenum source is seven
Ammonium molybdate or sodium molybdate, the substance withdrawl syndrome of molybdenum is 0.09-0.35mol/L, preferably 0.09-0.16mol/L.
5th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, wherein the sulphur source is optional
With thiocarbamide, thioacetamide or vulcanized sodium, the molal quantity of sulphur is 0.30-1.2mol/L.
6th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, molybdenum and sulphur rubs in raw material
You are than being 1: 2~1: 5；Preferably 1: 2.5-4.
7th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, molybdenum is lived with surface in raw material
Property agent monomer quality ratio for 1: 0.3~1: 5, preferably 1: 0.5-2.
8th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, wherein the reaction temperature
It is 150-240 DEG C, preferably 200 DEG C；Reaction time is 8-32h, preferably for 24 hours.
9th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, wherein the reaction under high pressure
Kettle is 100mL, and the compactedness of autoclave body is 40-80%；Preferably 70%.
10th, the preparation method of the controllable flower-shaped molybdenum disulfide hollow ball of size of the present invention, using be dried under reduced pressure, it is cold
Dry or vacuum drying is lyophilized, to reduce influence of the air to product.
The present invention has the following advantages：
(1) the flower-shaped hollow ball of molybdenum disulfide prepared by the present invention, spherical structure is complete, and flower-shaped lamella arrangements are loose, should
Structure large specific surface area and loose lamella arrangements not only contribute to exposing and being conducive to reactant to ball for catalytic active site
The internal surface area of shell diffusion inside and utilization spherical shell can provide a large amount of catalytic active site for catalysis reaction.
(2) the flower-shaped hollow ball of molybdenum disulfide for preparing of the present invention, the grain size and wall thickness of sphere be uniform, adjustable and with structure
Stablize, preferable stability can be provided for catalysis reaction.In the flower-shaped hollow ball of molybdenum disulfide a large amount of catalytic active site and preferably
Structural stability it is made to have in the catalytic fields such as electricity liberation of hydrogen, oil hydrogenation desulfurization, the hydrotreating of polycyclic aromatic hydrocarbon preferably
Application prospect.
(3) preparation process of the present invention is simple, low for equipment requirements, synthesizer is simple, and modulating method is simple, flow is simple
It is single, it is easy to operate；Raw material is easy to get at low cost, and reaction time is short, and product purity is high, and the yield of product is high.The preparation side of the present invention
Method is expected to be used for the adjustable transient metal sulfide of synthesis appearance structure and transition metal oxide.
The specific embodiment of the present invention is further described in conjunction with the following drawings.
Description of the drawings：
Fig. 1：The scanning electron microscope (SEM) of obtained flower-shaped hollow ball different amplification prepared by the embodiment of the present invention 1 is shone
Piece.
Fig. 2：The transmission electron microscope (TEM) of obtained flower-shaped hollow ball different amplification prepared by the embodiment of the present invention 1 shines
Piece.
Fig. 3 is the SEM figures of sample after roasting.
Fig. 4：The SEM figures of flower-shaped hollow ball prepared by embodiment 2-4.
Fig. 5：The TEM figures of flower-shaped hollow ball prepared by embodiment 2-4.
Specific embodiment
For the ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.
Embodiment 1
The CTAB of 0.14g is dissolved in the mixed solution of 70mL (VAbsolute ethyl alcohol/VWater=1/19) it after, stirring 30min, is mixing
1.70g (NH are added in solution4)6Mo7O24With 1.76g CS (NH2)2.Completely rear addition 2mL N to be dissolved2H4H2O makees reducing agent,
Solution is transferred in the reaction kettle of 100mL again, as in vacuum drying chamber, 200 DEG C of heat preservations for 24 hours, are cooled to room temperature.Reaction production
It after object is centrifuged, is washed respectively with deionized water and absolute ethyl alcohol, finally the dry 12h in 70 DEG C of vacuum drying chamber
Afterwards, gained sample is denoted as S-1.To detect the stability of the flower-shaped hollow ball structure of molybdenum disulfide, sample S-1 is placed in 400 DEG C, H2
After roasting 4h in atmosphere, gained sample is denoted as DS-1.
Fig. 1 schemes for flower-shaped hollow ball SEM.
Known by Fig. 1, sample is flower-shaped hollow ball, and spherical structure is complete, uniform particle diameter.Hollow ball is by molybdenum disulfide nano
Piece is accumulated, and particle size distribution range is about 1.2-1.5 μm or so narrow.Known by EDS data, mainly by Mo, S, C, O and N in sample
Element forms.The molar ratio of wherein Mo and S elements is 1：2.1, it is basically identical with the stoichiometric relationships of molybdenum disulfide.
Fig. 2 is the TEM pictures of flower-shaped hollow ball.As seen from the figure, flower-shaped hollow ball is assembled by molybdenum disulfide nano sheet
, the wall thickness of sphere is uniform, about 150nm or so.The length of nanometer sheet is in 20-60nm or so.
Fig. 3 is the SEM figures of sample after roasting.After roasting, flower-shaped hollow ball structure is complete, about 1.2-1.5 μm or so of grain size.
Sample before comparison roasting, the grain size pattern of sphere are basically identical.Therefore, the flower-shaped hollow-core construction of the sample has higher steady
It is qualitative.
Embodiment 2
The PEG of 0.20g is dissolved in the mixed solution of 70mL (VAbsolute ethyl alcohol/VWater=1/7) it is molten mixing after, stirring 30min
1.70g (NH are added in liquid4)6Mo7O24With 1.76g CS (NH2)2.Completely rear addition 2mL N to be dissolved2H4H2O makees reducing agent, then
Solution is transferred in the reaction kettle of 100mL, as in vacuum drying chamber, 200 DEG C of heat preservations for 24 hours, are cooled to room temperature.Reaction product
It after being centrifuged, is washed respectively with deionized water and absolute ethyl alcohol, finally the dry 12h in 70 DEG C of vacuum drying chamber.It dries
Gained sample is denoted as S-2 after dry.The structure of sample, component, pattern are basically identical with embodiment 1.
Embodiment 3
The CTAB of 0.05g is dissolved in the mixed solution of 70mL (VAbsolute ethyl alcohol/VWater=1/5) it is molten mixing after, stirring 30min
1.70g (NH are added in liquid4)6Mo7O24With 2.02g CS (NH2)2.Completely rear addition 2mL N to be dissolved2H4H2O makees reducing agent, then
Solution is transferred in the reaction kettle of 100mL, as in vacuum drying chamber, 200 DEG C of heat preservation 18h are cooled to room temperature.Reaction product
It after being centrifuged, is washed with deionized water and absolute ethyl alcohol, is finally dried for 24 hours in 50 DEG C of vacuum drying chamber respectively.It dries
Gained sample is denoted as S-3 after dry.The structure of sample, component, pattern are basically identical with embodiment 1.
Embodiment 4
The CTAB of 0.15g is dissolved in the mixed solution of 70mL (VAbsolute ethyl alcohol/VWater=7/13) it after, stirring 30min, is mixing
1.70g (NH are added in solution4)6Mo7O24With 1.76g CS (NH2)2.Completely rear addition 2mL N to be dissolved2H4H2O makees reducing agent,
Solution is transferred in the reaction kettle of 100mL again, as in vacuum drying chamber, 200 DEG C of heat preservations for 24 hours, are cooled to room temperature.Reaction production
It after object is centrifuged, is washed with deionized water and absolute ethyl alcohol, is finally dried for 24 hours in 50 DEG C of vacuum drying chamber respectively.
The product of gained is denoted as S-4 after drying.The structure of sample, component, pattern are basically identical with embodiment 1.
By the SEM and TEM of Fig. 4 and Fig. 5 it is found that sample prepared by embodiment 2-4 is flower-shaped hollow ball, which is by two
Molybdenum sulfide nanometer sheet is accumulated, and spherical structure is complete, and wall thickness is uniform.Its grain size is 1.2-2.2 μm, wall thickness 130-200nm.
With the increase of absolute ethyl alcohol and the volume ratio of water, the grain size of hollow ball increases in product, and wall thickness reduces.
Claims (10)
1. a kind of preparation method of the flower-shaped hollow ball of molybdenum disulfide, it is characterised in that：
(1) solution is prepared：Surfactant is dissolved in mixed solution, after stirring evenly, molybdenum source is added in and sulphur source is uniformly mixed
Afterwards, reducing agent N is added in2H4+H2O；
(2) it after the solution prepared in step (1) is stirred evenly, moves into reaction kettle, sealing is heated to 160-240 DEG C, constant temperature
It after reaction, is cooled to room temperature, obtains product；
(3) above-mentioned product is detached, after being washed respectively with water and absolute ethyl alcohol, vacuum drying obtains the flower-shaped hollow ball of molybdenum disulfide.
2. according to the method described in claim 1, it is characterized in that：The middle mixed solution using second alcohol and water of step (1) does molten
Agent, the volume ratio of second alcohol and water：0.01-0.6.
3. according to the method described in claim 1, it is characterized in that, using in surfactant CATB, PEG, PVP and SDS
One or two or more kinds, the substance withdrawl syndrome of surfactant is 3-10mmol/L in mixed solution.
4. according to the method described in claim 1, it is characterized in that：(NH can be selected in molybdenum source4)6Mo7O24Or one kind in sodium molybdate
Or two kinds, the substance withdrawl syndrome of molybdenum is 0.09-0.35mol/L in mixed solution.
5. according to the method described in claim 1, it is characterized in that：Sulphur source can be selected in thiocarbamide, thioacetamide, vulcanized sodium
One or two or more kinds, the amount of the substance of sulphur is 0.30-1.2mol/L in mixed solution.
6. according to the method described in claim 1,4 or 5, it is characterised in that：The molar ratio of molybdenum and sulphur is 1 in mixed solution：2-1
∶5。
7. according to the method described in claim 1,3 or 4, it is characterised in that：Molybdenum and surfactant monomer in mixed solution
Molar ratio is 1：0.3~1: 5.
8. according to the method described in claim 1, it is characterized in that, add in the 80%N that 2-5mL contents are2H4Aqueous solution.
9. according to the method described in claim 1, it is characterized in that, hydrothermal temperature is 160-240 DEG C, the hydro-thermal time is 8-32h,
The compactedness (stocking volume is autoclave body volume) of autoclave body is 40-80%.
10. according to the method described in claim 1, it is characterized in that, using being dried under reduced pressure, being freeze-dried or being dried in vacuo.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108715462A (en) * | 2018-08-31 | 2018-10-30 | 清华大学 | The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies |
| CN109638345A (en) * | 2018-12-18 | 2019-04-16 | 福州大学 | The method and its application in sodium-ion battery that one step hydro thermal method synthesizes graded structure hollow sphere |
| CN109650450A (en) * | 2019-01-18 | 2019-04-19 | 三峡大学 | A kind of hollow MoS2The preparation method and applications of microballoon |
| CN109908921A (en) * | 2019-03-11 | 2019-06-21 | 三峡大学 | A kind of MoS2/ NiO hollow microspheres, preparation method and application |
| CN110129112A (en) * | 2019-06-05 | 2019-08-16 | 青岛科技大学 | A kind of flower-shaped molybdenum disulfide/titanium dioxide nanometer composite particles ER fluid and preparation method thereof |
| CN110165155A (en) * | 2019-04-08 | 2019-08-23 | 陕西科技大学 | A kind of CNFs load MoS2The double salt cell positive materials of novel magnesium-lithium and its construction method |
| CN112786870A (en) * | 2021-02-10 | 2021-05-11 | 广西师范大学 | Polypyrrole coated MoS2/C composite material and preparation method thereof |
| CN115367802A (en) * | 2022-07-07 | 2022-11-22 | 河南科技大学 | Near-spherical molybdenum disulfide negative electrode material for lithium ion battery and preparation method thereof |
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| CN102701281A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of flower-shaped hollow molybdenum disulfide microspheres |
| CN105776335A (en) * | 2014-12-16 | 2016-07-20 | 中国石油天然气股份有限公司 | Preparation method of high-purity phase spherical nano molybdenum disulfide |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108715462A (en) * | 2018-08-31 | 2018-10-30 | 清华大学 | The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies |
| CN109638345A (en) * | 2018-12-18 | 2019-04-16 | 福州大学 | The method and its application in sodium-ion battery that one step hydro thermal method synthesizes graded structure hollow sphere |
| CN109638345B (en) * | 2018-12-18 | 2021-08-31 | 福州大学 | Method for synthesizing graded-structure hollow sphere by one-step hydrothermal method and application of graded-structure hollow sphere in sodium ion battery |
| CN109650450A (en) * | 2019-01-18 | 2019-04-19 | 三峡大学 | A kind of hollow MoS2The preparation method and applications of microballoon |
| CN109908921A (en) * | 2019-03-11 | 2019-06-21 | 三峡大学 | A kind of MoS2/ NiO hollow microspheres, preparation method and application |
| CN109908921B (en) * | 2019-03-11 | 2022-02-01 | 三峡大学 | MoS2NiO blankCore microsphere material, preparation method and application |
| CN110165155A (en) * | 2019-04-08 | 2019-08-23 | 陕西科技大学 | A kind of CNFs load MoS2The double salt cell positive materials of novel magnesium-lithium and its construction method |
| CN110165155B (en) * | 2019-04-08 | 2022-03-18 | 陕西科技大学 | CNFs load MoS2Magnesium-lithium double-salt battery positive electrode material and construction method thereof |
| CN110129112A (en) * | 2019-06-05 | 2019-08-16 | 青岛科技大学 | A kind of flower-shaped molybdenum disulfide/titanium dioxide nanometer composite particles ER fluid and preparation method thereof |
| CN112786870A (en) * | 2021-02-10 | 2021-05-11 | 广西师范大学 | Polypyrrole coated MoS2/C composite material and preparation method thereof |
| CN115367802A (en) * | 2022-07-07 | 2022-11-22 | 河南科技大学 | Near-spherical molybdenum disulfide negative electrode material for lithium ion battery and preparation method thereof |
| CN115367802B (en) * | 2022-07-07 | 2024-02-23 | 河南科技大学 | Near-spherical molybdenum disulfide negative electrode material for lithium ion battery and preparation method thereof |
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Application publication date: 20180608 |