CN102701281A - Preparation method of flower-shaped hollow molybdenum disulfide microspheres - Google Patents
Preparation method of flower-shaped hollow molybdenum disulfide microspheres Download PDFInfo
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- CN102701281A CN102701281A CN2012101481442A CN201210148144A CN102701281A CN 102701281 A CN102701281 A CN 102701281A CN 2012101481442 A CN2012101481442 A CN 2012101481442A CN 201210148144 A CN201210148144 A CN 201210148144A CN 102701281 A CN102701281 A CN 102701281A
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Abstract
The invention relates to a preparation method of flower-shaped hollow molybdenum disulfide microspheres, belonging to the technical field of nanometer material preparation. The method provided by the invention comprises the following steps of: (1) solution preparation: dissolving (NH4)2MoO4, CS(NH2)2, NH2OH.HCl and a surfactant into water, dissolving to obtain the solution, and then adjusting the pH value to 5-6.5 by acid; (2) agitating the solution obtained in step (1), and then transferring to a reaction kettle, sealing and reacting at a constant temperature, and then cooling to the room temperature to obtain the reaction product; (3) separating the reaction product, washing and drying to obtain the flower-shaped hollow molybdenum disulfide microspheres. The shape of the flower-shaped hollow molybdenum disulfide microspheres prepared by the method provided by the invention is controllable. The method provided by the invention is simple in process and low in cost; the prepared product is high in purity and high in yield, has an important application in the field of tribology and photochemistry, and is expected to be applied to large-scale industrial production.
Description
Technical field
The invention belongs to the nano material preparation technical field, 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 advantages such as density is little, specific surface area is big, it has the potential application prospect in fields such as packing material, medicine transmission, 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 be used as the cathode material etc. of photochromics, catalyzer, lubricant, high energy battery.
Molybdenumdisulphide (MoS
2) have a laminate structure of similar graphite; Belonging to hexagonal system, is a kind of compound with diamagnetism and semiconductor property, and Mo-S faceted pebble specific surface area is big in its structure; In the layer is very strong covalent linkage; Interlayer then is more weak Van der Waals Er Sili, and layer is easy to peel off with layer, has good anisotropy and lower frictional coefficient.MoS with nanostructure
2On many performances, have been further upgraded; Show the following aspects highlightedly: specific surface area is very big, and adsorptive power is stronger, and reactive behavior is high; The catalytic performance especially performance of catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalytic material and air storage material; Nanometer MoS
2Thin layer can be with the nearly 1.78eV of differential, be complementary with the energy of light, on the sensitive cell material, application prospect is arranged; Along with MoS
2Particle diameter diminish, it all obviously improves in the tack of friction material surface and level of coverage, wear-resistant, antifriction performance is also significantly improved.
Up to now, people have carried out big quantity research in synthesizing 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 the hydro-thermal synthetic technology is applied to inorganic micro Nano material syntheticly has mild condition, simple to operate, pattern is prone to control, percent crystallinity advantages of higher.
It is less to adopt the elevated temperature heat reaction method to prepare the bibliographical information of flower-shaped MoS2 microballoon, and cost is high, complex process; Though and the low temperature method cost is lower, mostly the prepared MoS2 that obtains is one-dimentional structure or soccerballene shape Nano microsphere, adopts report that low temperature prepares flower-shaped molybdenumdisulphide tiny balloon seldom.
CN101113021A discloses a kind of compound method of flower-shaped molybdenum disulfide micro-balloon.This method is with Na
2MoO
4, CS (NH
2)
2Add reaction kettle with inorganic additives,, made in 12 hours in 150 ℃～250 ℃ reactions of thermostat container inner control temperature with deionized water dissolving and sealing.
CN101880061A discloses a kind of preparation method of inorganic fullerene molybdenum disulphide.This method adopts microemulsion method to prepare presoma MoS
3, and then in nitrogen and the hydrogen atmosphere to presoma MoS
3Heat-treat, prepare inorganic fullerene molybdenum disulphide.Characterize through high-resolution-ration transmission electric-lens, the molybdenumdisulphide that makes has fullerene structure, and median size is about 100nm.
But because nanoparticle is reunited in the preparation process easily, the molybdenumdisulphide tiny balloon pattern that prior art obtains is wayward, and prior art processes is complicated, influences its mass-producing in fields such as tribology, photochemistry and uses.
Summary of the invention
To the deficiency of prior art, one of the object of the invention is to provide a kind of preparation method of flower-shaped molybdenumdisulphide tiny balloon.
The present invention adopts hydrothermal synthesis method, and the preparation method of said flower-shaped molybdenumdisulphide tiny balloon may further comprise the steps:
(1) obtain solution: with (NH
4)
2MoO
4, CS (NH
2)
2, NH
2OHHCl and tensio-active agent are soluble in water, and dissolving obtains solution, and the pH value that uses acid-conditioning solution again is 5～6.5;
(2) after the solution stirring that step (1) is obtained, move into stainless steel cauldron, sealing after the isothermal reaction, is cooled to room temperature, obtains reaction product;
(3) separate above-mentioned reaction product, washing, drying obtain flower-shaped molybdenumdisulphide tiny balloon.
(NH
4)
2MoO
4Be molybdenum source, CS (NH
2)
2Be sulphur source, (NH
4)
2MoO
4With CS (NH
2)
2Reaction generates ammonium thiomolybdate, NH
2OHHCl reacts as reductive agent and ammonium thiomolybdate, obtains molybdenumdisulphide.Said (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; For example 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; Preferred 1.0～1.5: 3.0～4.5: 2.0～2.5, further preferred 1: 3: 2.
Tensio-active agent can play the effect that suppresses nanoparticle agglomerates as dispersion agent.Said tensio-active agent and (NH
4)
2MoO
4The ratio of amount of substance be 1: 4～8, for example 1: 4.5,1: 5,1: 5.5,1: 6,1: 6.5,1: 7,1: 7.5, preferred 1: 5～8, further preferred 1: 5.Said tensio-active agent is selected from non-ionics or/and cats product.Said non-ionics, cats product do not have concrete restriction, and the non-ionics that those skilled in the art can be known, cats product all can be realized the present invention.For example can select non-ionics F127 for use, cats product benzyltriethylammoinium chloride (C
13H
22ClN).F127 is 11500 polymer with 7: 3 composition of proportions molecular weight by T 46155 and polyoxypropylene.
Need the pH value with acid-conditioning solution among the present invention, wherein, said acid is hydrochloric acid, and the amount concentration of preferred substance is the hydrochloric acid of 2mol/L.
The time of said stirring is 20～50min, for example 22min, 24min, 26min, 28min, 48min, 46min, 44min, preferred 25～45min, further preferred 30min.The temperature of said isothermal reaction is 140 ℃～200 ℃, for example 145 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 185 ℃, 195 ℃, and preferred 180 ℃～200 ℃, further preferred 180 ℃.
The time of isothermal reaction is 24h at least, for example 25h, 25.5h, 26h, 26.5h, 27h, 27.5h, 28h, 28.5h, 29h, 29.5h, 35h, 38h, preferred 24h～30h, further preferred 24h.
Preferred said isothermal reaction is carried out under vacuum condition.
The volume of said water is 60%～90% of a reaction kettle volume, for example 62%, 64%, 66%, 68%, 88%, 86%, 84%, 82%, and preferred 60%～80%, further preferred 70%.
The mode of said sealing is restriction not, and any mode that can reach sealed reactor that those skilled in the art can be known all can realize the present invention, for example, can adopt teflon seal among the present invention.
Said separation is selected from the combination of a kind of in filtration, deposition, centrifugal, the distillation or at least two kinds.Said combination for example precipitates and filtering combination, filters and the centrifugal combination, and centrifugal and distillatory combination, filtration, deposition and centrifugal combination, deposition, centrifugal and distillatory combination, preferably centrifugal and filtering combination, further preferably centrifugal.
Those skilled in the art can select cleaning solvent based on the knowledge of oneself grasping, and among the present invention, as preferred version, deionized water and absolute ethanol washing are adopted in said washing.
Preferably; Said drying is selected from the combination of a kind of in spraying drying, forced air drying, microwave drying, infrared drying, the vacuum-drying or at least two kinds, and said combination is the combination of spraying drying and forced air drying for example, 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 preferred vacuum-drying.
Preferably, said vacuum drying temperature is 50 ℃～90 ℃, preferred 60～80 ℃, and further preferred 80 ℃.
Another object of the present invention is to provide a kind of flower-shaped molybdenumdisulphide tiny balloon that is obtained by method for preparing, it is the flower-shaped tiny balloon of 1～2 μ m for diameter.
The ball edge of the flower-shaped molybdenumdisulphide tiny balloon for preparing through the present invention is a flower-like structure, and laminate structure is obvious.
The inventive method technology is simple, and is with low cost, and the product purity for preparing is high, productive rate is high, and in fields such as tribology, photochemistry, has important use, is expected to be used 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, the present invention has following advantage:
(1) the present invention adopts one step hydro thermal method synthetic, and introduces tensio-active agent, has simplified process step, and cost is inexpensive, and production technique is simple and easy to control, is fit to large-scale industrial production.
(2) the present invention selects NH for use
2OHHCl is a reductive agent, and in reaction, it is oxidized to gases such as nitrogen, water and nitrogen protoxide, can not bring impurity to reaction, has improved the purity of final product;
(3) adding of tensio-active agent can be controlled flower-shaped molybdenumdisulphide tiny balloon pattern among the present invention, and laminate structure is obvious, and has higher specific surface area and frictional behaviour.
Description of drawings
Be further described below in conjunction with the accompanying drawing specific embodiments of the invention.
Fig. 1: the flower-shaped molybdenumdisulphide tiny balloon XRD spectra that the embodiment of the invention 1 prepares;
Fig. 2: the flower-shaped molybdenumdisulphide tiny balloon Electronic Speculum ability spectrogram (EDX) that the embodiment of the 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 invention 1 prepares;
Fig. 4: transmission electron microscope (TEM) photo of the flower-shaped molybdenumdisulphide tiny balloon different amplification that the embodiment of the invention 1 prepares.
Embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment helps to understand the present invention, should not be regarded as concrete restriction of the present invention.Can know that by technological general knowledge the present invention also can describe through other the scheme that does not break away from technical characterictic of the present invention, thus all within the scope of the present invention or the change that is equal in the scope of the invention all comprised by the present invention.
Embodiment 1:
With 0.2g C
13H
22ClN is dissolved in the zero(ppm) water of 70ml, adds 1.40g CS (NH then
2)
2, 0.725gNH
2OHHCl and 0.88g (NH
4)
2MoO
4After treating to dissolve fully, use 2molL again
-1HCl regulate about pH value to 6.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 24h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, promptly flower-shaped molybdenumdisulphide tiny balloon.
Fig. 1 is flower-shaped molybdenumdisulphide tiny balloon XRD spectra, all diffraction peaks all with pure MoS
2Crystal standard diffractogram (PDF No.37-1492) unanimity of six side's phases.Therefore, the hydro-thermal reaction synthetic should be the MoS of nanoscale
2The EDX of Fig. 2 analyzes in this globe of surface and only has Mo and S, and further specifying the synthetic product is MoS
2Fig. 3 is the SEM figure of product, from figure, can see the flower-shaped MoS of a large amount of homogeneous
2Microballoon, wherein some tiny balloon growth not exclusively the pattern of ball in midair occurs.Fig. 4 is the TEM figure of product, and further specifying synthetic of the present invention is the flower-shaped MoS that diameter is about 1～2um
2Tiny balloon, the ball edge is a flower-like structure, and laminate structure is obvious.
Embodiment 2:
13.6g F127 is dissolved in the zero(ppm) water of 70ml, adds 1.40g CS (NH then
2)
2, 0.725gNH
2OHHCl and 0.88g (NH
4)
2MoO
4After treating to dissolve fully, use 2molL again
-1HCl regulate about pH value to 6.After stirring 30min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 24h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, promptly flower-shaped molybdenumdisulphide tiny balloon.
With 0.383g (C
8H
17)
2(CH
3)
2NCl is dissolved in the zero(ppm) water of 60ml, adds 2.28gCS (NH then
2)
2, 1.45g NH
2OHHCl and 1.01g (NH
4)
2MoO
4After treating to dissolve fully, use 2molL again
-1HCl regulate about pH value to 5.After stirring 20min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 140 ℃ of insulation 30h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after filtering separation, forced air drying obtains the product powder of grey black, promptly flower-shaped molybdenumdisulphide tiny balloon.
With 0.057g (C
8H
17)
2(CH
3)
2NCl is dissolved in the zero(ppm) water of 90ml, adds 0.381gCS (NH then
2)
2, 0.218g NH
2OHHCl and 0.303g (NH
4)
2MoO
4After treating to dissolve fully, use 2molL again
-1HCl regulate about pH value to 6.5.After stirring 50min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 28h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after precipitate and separate, microwave drying obtains the product powder of grey black, promptly flower-shaped molybdenumdisulphide tiny balloon.
With 0.061gC
13H
22ClN is dissolved in the zero(ppm) water of 80ml, adds 0.228g CS (NH then
2)
2, 0.145gNH
2OHHCl and 0.2020.057g (NH
4)
2MoO
4After treating to dissolve fully, use 2molL again
-1HCl regulate about pH value to 5.5.After stirring 40min, mixed solution is transferred in the stainless steel cauldron of 100ml, places vacuum drying oven, be cooled to room temperature in 180 ℃ of insulation 32h.Reaction product is used deionized water and absolute ethyl alcohol repetitive scrubbing respectively after spinning, infrared drying obtains the product powder of grey black, promptly flower-shaped molybdenumdisulphide tiny balloon.
Applicant's statement; The present invention explains detailed process equipment of the present invention and technical process through the foregoing description; But the present invention is not limited to above-mentioned detailed process equipment and technical process, does not mean that promptly the present invention must rely on above-mentioned detailed process equipment and technical process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. the preparation method of a flower-shaped molybdenumdisulphide tiny balloon is characterized in that, said method comprising the steps of:
(1) obtain solution: with (NH
4)
2MoO
4, CS (NH
2)
2, NH
2OHHCl and tensio-active agent are soluble in water, and dissolving obtains solution, and the pH value that uses acid-conditioning solution again is 5～6.5;
(2) after the solution stirring that step (1) is obtained, move into stainless steel cauldron, sealing after the isothermal reaction, is cooled to room temperature, obtains reaction product;
(3) separate above-mentioned reaction product, washing, drying obtain flower-shaped molybdenumdisulphide tiny balloon.
2. method according to claim 1 is characterized in that, said (NH
4)
2MoO
4, CS (NH
2)
2, NH
2The ratio of the amount of substance of OHHCl is 0.5～1.5: 3.0～5.0: 2.0～3.0, preferred 1.0～1.5: 3.0～4.5: 2.0～2.5, and further preferred 1: 3: 2.
3. method according to claim 1 and 2 is characterized in that, said tensio-active agent and (NH
4)
2MoO
4The ratio of amount of substance be 1: 4～8, preferred 1: 5～8, preferred 1: 5;
Preferably, said tensio-active agent is selected from non-ionics or/and cats product.
4. according to each described method of claim 1-3, it is characterized in that said acid is hydrochloric acid, the amount concentration of preferred substance is the hydrochloric acid of 2mol/L.
5. according to each described method of claim 1-4, it is characterized in that said churning time is 20～50min, preferred 25～45min, further preferred 30min;
Preferably, the temperature of said isothermal reaction is 140 ℃～200 ℃, preferred 180 ℃～200 ℃, and further preferred 180 ℃.
6. according to each described method of claim 1-5, it is characterized in that the time of said isothermal reaction is 24h at least, preferred 24h～30h, further preferred 24h;
Preferably, said isothermal reaction is carried out under vacuum condition.
7. according to each described method of claim 1-6, it is characterized in that the volume of said water is 60%～90% of a reaction kettle volume, preferred 60%～80%, further preferred 70%.
8. according to each described method of claim 1-7, it is characterized in that said separation is selected from the combination of a kind of in filtration, deposition, centrifugal, the distillation or at least two kinds, preferred centrifugal and filtering combination is further preferably centrifugal;
Preferably, deionized water and absolute ethanol washing are adopted in said washing.
9. according to each described method of claim 1-8; It is characterized in that; Said drying is selected from the combination of a kind of in spraying drying, forced air drying, microwave drying, infrared drying, the vacuum-drying or at least two kinds; The combination of preferred vacuum-drying and forced air drying, further preferred vacuum-drying;
Preferably, said vacuum drying temperature is 50 ℃～90 ℃, preferred 60～80 ℃, and further preferred 80 ℃.
10. a flower-shaped molybdenumdisulphide tiny balloon that is prepared by each said method of claim 1-9 is characterized in that, it is the flower-shaped tiny balloon of 1～2 μ m for diameter.
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