CN102701281B - A kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon - Google Patents
A kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon Download PDFInfo
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- CN102701281B CN102701281B CN201210148144.2A CN201210148144A CN102701281B CN 102701281 B CN102701281 B CN 102701281B CN 201210148144 A CN201210148144 A CN 201210148144A CN 102701281 B CN102701281 B CN 102701281B
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Abstract
The present invention relates to a kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon, belong to technical field of nanometer material preparation.The method of the invention comprises the following steps: (1) obtain solution: by (NH
4)
2moO
4, CS (NH
2)
2, NH
2oHHCl and tensio-active agent soluble in water, dissolving and obtain solution, then is 5 ~ 6.5 by the pH value of acid-conditioning solution; (2) after solution stirring step (1) obtained, move into reactor, sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product; (3) be separated above-mentioned reaction product, washing, drying, obtain flower-shaped molybdenumdisulphide tiny balloon.By the flower-shaped molybdenumdisulphide tiny balloon morphology controllable that the method for the invention prepares.The inventive method technique is simple, and with low cost, the product purity prepared is high, productive rate is high, and has important application in the field such as tribology, photochemistry, is expected to for large-scale industrial production.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly, the present invention relates to a kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon.
Background technology
Nano structural material has unique physics, chemistry, electricity, magnetics and mechanical property.Because it has the advantages such as density is little, specific surface area is large, it has potential application prospect in fields such as packing material, drug delivery, catalysis.Therefore, carry out the preparation research of this type of material, have very important significance.Existing research shows, the disulphide of transition metal has unique character, and they can as the cathode material etc. of photochromics, catalyzer, lubricant, high energy battery.
Molybdenumdisulphide (MoS
2) there is the laminate structure of similar graphite, belong to hexagonal system, it is a kind of compound with diamagnetism and semiconductor property, in its structure, Mo-S faceted pebble specific surface area is large, very strong covalent linkage in layer, interlayer is then more weak Van der Waals Er Sili, and layer and layer are easy to peel off, and has good anisotropy and lower frictional coefficient.There is the MoS of nanostructure
2many performances are had been further upgraded, show the following aspects highlightedly: specific surface area is very big, adsorptive power is stronger, and reactive behavior is high, the performance of catalytic performance especially catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalytic material and gas storing material; Nanometer MoS
2thin layer can be with the nearly 1.78eV of differential, match with the energy of light, photocell material have application prospect; Along with MoS
2particle diameter diminish, it all significantly improves in the tack of friction material surface and level of coverage, and wear-resistant, antifriction performance is also significantly improved.
Up to now, people have carried out large quantity research in the synthesis of molybdenum disulfide nano material, mainly contain high temperature solid state reaction, thermal decomposition method, high-temperature gas-solid reaction, vapour deposition process, hydrothermal method etc.Wherein Hydrothermal Synthesis technology be applied to inorganic micro Nano material synthesis has mild condition, simple to operate, pattern is easily controlled, degree of crystallinity advantages of higher.
The bibliographical information that employing high-temperature hot reaction method prepares flower-shaped MoS2 microballoon is less, and cost is high, complex process; And although low temperature method cost is lower, preparation-obtained MoS2 mostly is one-dimentional structure or soccerballene shape Nano microsphere, adopts the report of low-temperature growth flower-shaped molybdenumdisulphide tiny balloon little.
CN101113021A discloses a kind of synthetic method of flower-shaped molybdenum disulfide micro-balloon.The method is by Na
2moO
4, CS (NH
2)
2add reactor with inorganic additives, seal with deionized water dissolving, in thermostat container, control temperature 150 DEG C ~ 250 DEG C reaction obtains for 12 hours.
CN101880061A discloses a kind of preparation method of inorganic fullerene molybdenum disulphide.The method adopts microemulsion method to prepare presoma MoS
3, and then to presoma MoS in nitrogen and hydrogen atmosphere
3heat-treat, prepare inorganic fullerene molybdenum disulphide.Characterize through high-resolution-ration transmission electric-lens, obtained molybdenumdisulphide has fullerene structure, and median size is at about 100nm.
But because nanoparticle is easily reunited in preparation process, the molybdenumdisulphide tiny balloon pattern that prior art obtains is wayward, and prior art processes is complicated, affect its in the field such as tribology, photochemistry mass-producing application.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the preparation method providing a kind of flower-shaped molybdenumdisulphide tiny balloon.
The present invention adopts hydrothermal synthesis method, and the preparation method of described flower-shaped molybdenumdisulphide tiny balloon comprises the following steps:
(1) obtain solution: by (NH
4)
2moO
4, CS (NH
2)
2, NH
2oHHCl and tensio-active agent soluble in water, dissolving and obtain solution, then is 5 ~ 6.5 with the pH value of acid-conditioning solution;
(2) after solution stirring step (1) obtained, move into stainless steel cauldron, sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product;
(3) be separated above-mentioned reaction product, washing, drying, obtain flower-shaped molybdenumdisulphide tiny balloon.
(NH
4)
2moO
4for molybdenum source, CS (NH
2)
2for sulphur source, (NH
4)
2moO
4with CS (NH
2)
2reaction generates ammonium thiomolybdate, NH
2oHHCl reacts as reductive agent and ammonium thiomolybdate, obtains molybdenumdisulphide.Described (NH
4)
2moO
4, CS (NH
2)
2, NH
2the ratio of OHHCl amount of substance is 0.5 ~ 1.5: 3.0 ~ 5.0: 2.0 ~ 3.0, such as 0.6: 3.1: 2.1,0.7: 3.2: 2.2,0.7: 3.3: 2.3,1.4: 4.9: 2.9,1.2: 4.8: 2.8,1.1: 4.6: 2.6, preferably 1.0 ~ 1.5: 3.0 ~ 4.5: 2.0 ~ 2.5, further preferably 1: 3: 2.
Tensio-active agent, as dispersion agent, can play the effect suppressing nanoparticle agglomerates.Described tensio-active agent and (NH
4)
2moO
4the ratio of amount of substance be 1: 4 ~ 8, such as 1: 4.5,1: 5,1: 5.5,1: 6,1: 6.5,1: 7,1: 7.5, preferably 1: 5 ~ 8, further preferably 1: 5.Described tensio-active agent is selected from nonionic surface active agent or/and cats product.The restriction that described nonionic surface active agent, cats product are not concrete, nonionic surface active agent, cats product that those skilled in the art can be known all can realize the present invention.Such as can select nonionic surface active agent F127, cats product benzyltriethylammoinium chloride (C
13h
22clN).F127 by polyoxyethylene and polyoxypropylene with 7: 3 composition of proportions molecular weight be the polymer of 11500.
Need the pH value with acid-conditioning solution in the present invention, wherein, described acid is hydrochloric acid, and the amount concentration of preferred substance is the hydrochloric acid of 2mol/L.
The time of described stirring is 20 ~ 50min, such as 22min, 24min, 26min, 28min, 48min, 46min, 44min, preferably 25 ~ 45min, further preferred 30min.The temperature of described isothermal reaction is 140 DEG C ~ 200 DEG C, such as 145 DEG C, 155 DEG C, 160 DEG C, 165 DEG C, 170 DEG C, 175 DEG C, 185 DEG C, 195 DEG C, preferably 180 DEG C ~ 200 DEG C, preferably 180 DEG C further.
Time of isothermal reaction is at least 24h, such as 25h, 25.5h, 26h, 26.5h, 27h, 27.5h, 28h, 28.5h, 29h, 29.5h, 35h, 38h, preferred 24h ~ 30h, further preferred 24h.
Preferred described isothermal reaction is carried out under vacuum.
The volume of described water is 60% ~ 90% of reactor volume, such as 62%, 64%, 66%, 68%, 88%, 86%, 84%, 82%, preferably 60% ~ 80%, further preferably 70%.
The mode of described sealing does not limit, and any mode that can reach sealed reactor that those skilled in the art can be known all can realize the present invention, such as, can adopt teflon seal in the present invention.
Described separation is selected from a kind of or combination of at least two kinds in filtration, precipitation, centrifugal, distillation.The combination that described combination such as precipitates and filters, filters and centrifugal combination, the combination of centrifugal and distillation, filters, precipitation and centrifugal combination, the combination of precipitation, centrifugal and distillation, the combination of preferably centrifugal and filtration, preferably centrifugal further.
The knowledge-chosen cleaning solvent that those skilled in the art can grasp according to oneself, in the present invention, preferably, described washing adopts deionized water and absolute ethanol washing.
Preferably, described drying is selected from the combination of a kind of in spraying dry, forced air drying, microwave drying, infrared drying, vacuum-drying or at least two kinds, the combination of described combination such as spraying dry and forced air drying, the combination of forced air drying and microwave drying, the combination of microwave drying and infrared drying, infrared drying and vacuum drying combination, the combination of preferred vacuum-drying and forced air drying, further preferably vacuum-drying.
Preferably, described vacuum drying temperature is 50 DEG C ~ 90 DEG C, preferably 60 ~ 80 DEG C, preferably 80 DEG C further.
Another object of the present invention is to provide a kind of flower-shaped molybdenumdisulphide tiny balloon prepared by aforesaid method, its for diameter be the flower-shaped tiny balloon of 1 ~ 2 μm.
The ball edge of the flower-shaped molybdenumdisulphide tiny balloon prepared by the present invention is flower-like structure, and laminate structure is obvious.
The inventive method technique is simple, and with low cost, the product purity prepared is high, productive rate is high, and has important application in the field such as tribology, photochemistry, is expected to for large-scale industrial production.
The present invention introduces tensio-active agent and replaces inorganic additives, and molybdenumdisulphide tiny balloon pattern is more easy to control, and has higher specific surface area and tribological property.
Compared with prior art, tool of the present invention has the following advantages:
(1) the present invention adopts one step hydro thermal method to synthesize, and introduces tensio-active agent, and simplify processing step, cost is inexpensive, and production technique is simple and easy to control, is applicable to large-scale industrial production.
(2) the present invention selects NH
2oHHCl is reductive agent, and in the reaction, it is oxidized to the gases such as nitrogen, water and nitrogen protoxide, can not bring impurity, improve the purity of final product to reaction;
(3) in the present invention, adding of tensio-active agent makes flower-shaped molybdenumdisulphide tiny balloon pattern control, and laminate structure is obvious, and has higher specific surface area and frictional behaviour.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described.
Fig. 1: the flower-shaped molybdenumdisulphide tiny balloon XRD spectra that the embodiment of the present invention 1 prepares;
Fig. 2: flower-shaped molybdenumdisulphide tiny balloon electro microscope energy spectrum figure (EDX) that the embodiment of the present invention 1 prepares;
Fig. 3: field scan Electronic Speculum (SEM) photo of the flower-shaped molybdenumdisulphide tiny balloon different amplification that the embodiment of the present invention 1 prepares;
Fig. 4: transmission electron microscope (TEM) photo of the flower-shaped molybdenumdisulphide tiny balloon different amplification that the embodiment of the present invention 1 prepares.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.As known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1:
By 0.2g C
13h
22clN is dissolved in the distilled water of 70ml, then adds 1.40g CS (NH
2)
2, 0.725gNH
2oHHCl and 0.88g (NH
4)
2moO
4.Until completely dissolved, then use 2molL
-1hCl adjust ph to 6 about.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 24h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. flower-shaped molybdenumdisulphide tiny balloon.
Fig. 1 is flower-shaped molybdenumdisulphide tiny balloon XRD spectra, all diffraction peaks all with pure MoS
2the crystal standard diffraction figure (PDF No.37-1492) of six side's phases is consistent.Therefore, that hydro-thermal reaction synthesis should be the MoS of nanoscale
2.The EDX of Fig. 2 analyzes in this globe of surface only exists Mo and S, and the product further illustrating synthesis is MoS
2.Fig. 3 is the SEM figure of product, flower-shaped MoS homogeneous in a large number as we can see from the figure
2microballoon, wherein the growth of some tiny balloon not exclusively, occurs the pattern of ball in midair.Fig. 4 is the TEM figure of product, and that further illustrate the present invention's synthesis is the flower-shaped MoS that diameter is about 1 ~ 2um
2tiny balloon, ball edge is flower-like structure, and laminate structure is obvious.
Embodiment 2:
13.6g F127 is dissolved in the distilled water of 70ml, then adds 1.40g CS (NH
2)
2, 0.725gNH
2oHHCl and 0.88g (NH
4)
2moO
4.Until completely dissolved, then use 2molL
-1hCl adjust ph to 6 about.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 24h, is cooled to room temperature.Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. flower-shaped molybdenumdisulphide tiny balloon.
Embodiment 3
By 0.383g (C
8h
17)
2(CH
3)
2nCl is dissolved in the distilled water of 60ml, then adds 2.28gCS (NH
2)
2, 1.45g NH
2oHHCl and 1.01g (NH
4)
2moO
4.Until completely dissolved, then use 2molL
-1hCl adjust ph to 5 about.After stirring 20min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 140 DEG C of insulation 30h, is cooled to room temperature.After reaction product is separated by filtration, use deionized water and dehydrated alcohol repetitive scrubbing respectively, forced air drying obtains the powder product of grey black, i.e. flower-shaped molybdenumdisulphide tiny balloon.
Embodiment 4
By 0.057g (C
8h
17)
2(CH
3)
2nCl is dissolved in the distilled water of 90ml, then adds 0.381gCS (NH
2)
2, 0.218g NH
2oHHCl and 0.303g (NH
4)
2moO
4.Until completely dissolved, then use 2molL
-1hCl adjust ph to 6.5 about.After stirring 50min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 28h, is cooled to room temperature.Reaction product is after precipitate and separate, and use deionized water and dehydrated alcohol repetitive scrubbing respectively, microwave drying obtains the powder product of grey black, i.e. flower-shaped molybdenumdisulphide tiny balloon.
Embodiment 5
By 0.061gC
13h
22clN is dissolved in the distilled water of 80ml, then adds 0.228g CS (NH
2)
2, 0.145gNH
2oHHCl and 0.2020.057g (NH
4)
2moO
4.Until completely dissolved, then use 2molL
-1hCl regulate about pH value to 5.5.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying oven in 180 DEG C of insulation 32h, is cooled to room temperature.Reaction product is after centrifugation, and use deionized water and dehydrated alcohol repetitive scrubbing respectively, infrared drying obtains the powder product of grey black, i.e. flower-shaped molybdenumdisulphide tiny balloon.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (1)
1. a preparation method for flower-shaped molybdenumdisulphide tiny balloon, is characterized in that, said method comprising the steps of:
By 0.2g C
13h
22clN is dissolved in the distilled water of 70mL, then adds 1.40g CS (NH
2)
2, 0.725gNH
2oHHCl and 0.88g (NH
4)
2moO
4, until completely dissolved, then use 2molL
-1hCl adjust ph to 6; After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100mL, is placed in vacuum drying oven in 180 DEG C of insulation 24h, is cooled to room temperature; Reaction product, after centrifugation, uses deionized water and dehydrated alcohol repetitive scrubbing respectively, and finally 80 DEG C of dry 10h obtain the powder product of grey black under vacuum, i.e. flower-shaped molybdenumdisulphide tiny balloon.
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| 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 |
| CN112680955B (en) * | 2020-12-20 | 2022-11-11 | 江苏纳盾科技有限公司 | Photo-thermal conversion textile based on self-assembled molybdenum disulfide nanospheres and preparation method thereof |
| CN115744990A (en) * | 2022-11-24 | 2023-03-07 | 南昌大学 | Method for thermally synthesizing multi-morphology nano molybdenum disulfide lubricant additive by water/solvent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024517A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Method for preparing non-crystal molybdemum sulfide nano powder |
| CN101113021A (en) * | 2007-07-03 | 2008-01-30 | 浙江大学 | Method for preparing flower-shaped molybdenum disulfide micro-balloon |
-
2012
- 2012-05-14 CN CN201210148144.2A patent/CN102701281B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024517A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Method for preparing non-crystal molybdemum sulfide nano powder |
| CN101113021A (en) * | 2007-07-03 | 2008-01-30 | 浙江大学 | Method for preparing flower-shaped molybdenum disulfide micro-balloon |
Non-Patent Citations (3)
| Title |
|---|
| "MoS2纳米花的溶剂热合成及其表征";孙燕丽等;《无机化学学报》;20080630;第24卷(第6期);第1003-1006页 * |
| "Study on Hydrothermal Synthesis of Flower-sphere MoS2";Jun Zhou et al.;《Advanced Materials Research》;20110816;第311-313卷;第566-570页 * |
| "水热法制备二硫化钼微球花及其结构表征";任萍等;《有色金属(冶炼部分)》;20111231(第10期);第47-49、53页 * |
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