CN106044856B - The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in coupling is sanded in ultrasound - Google Patents
The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in coupling is sanded in ultrasound Download PDFInfo
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Abstract
The invention belongs to nano material processing technique field, and in particular to the method for coupling stripping preparing molybdenum disulfide from molybdenite nanometer sheet is sanded to a kind of ultrasound.This method comprises the following steps：1）Molybdenite micro mist is scattered in peel off in solvent and forms suspension；2）Dispersant, stripping auxiliary agent are dissolved in step 1）Suspension in ultrasonic disperse；3）Step 2）Continuous peel off obtains molybdenum disulfide nano sheet to suspension after ultrasonic disperse under ultrasound, sand milling coupling simultaneously." ultrasound is sanded " coupling that the present invention designs peels off new method stripping molybdenite micro mist and prepares molybdenum disulfide nano sheet on a large scale, realizes the green conversion from natural minerals to performance function material, has significant application value and economic benefit.
Description
Technical field
The invention belongs to nano material processing technique field, and in particular to peel off molybdenite to a kind of ultrasound-sand milling coupling
The method for preparing molybdenum disulfide nano sheet.
Background technology
MoS2Nanometer sheet and its composite have abundant physicochemical characteristics, in catalysis, energy conversion and storage, ring
There is important application in the fields such as border purification, lubrication.Block MoS2For indirect gap semiconductor（E g=1.2 eV）, and its single layer structure is then
Be changed into energy gap be 1.8 eV direct gap semiconductor [Nano Lett.2011,11,5111-5116], have fluorescence special
Property, biological label agent, and efficient sun light absorber can be made.Especially, MoS2It is nanocrystalline to produce hydrogen with excellent electro-catalysis
Catalytic performance, be expected to the part substitution noble metal such as Pt, will be greatly reduced use cost [Nano Lett. 2014, 14,
553-558].In addition, MoS2Based nano composite material can do lithium（Sodium）Ion battery electrode [ACS Appl. Mater. Interfaces2014, 6, 7084-7089].Few layer MoS2Nanometer sheet（Few-layer MoS2nanoplates）It is controllable
Prepared by magnanimity and its performance regulation and control are focus and the forward position of current international research.
Inexpensively, the preparation MoS of the controllable magnanimity of green2Nanometer sheet sill has most important theories and application value.MoS at present2
The preparation of nanometer sheet mainly has two kinds：From bottom to top with approach from top to bottom.Approach includes hydro-thermal, chemical vapor deposition from bottom to top
The methods of product, thermal decomposition [Electrochimica Acta. 2014, 132, 397-403; Scientific reports,
2013, 3, 1866-1871; Small, 2012,8,966-971], it is pattern easy-regulating the characteristics of these methods, but
Equipment, process are complicated, and condition is harsh, it is difficult to produces in enormous quantities.From top to bottom approach include micromechanics stripping, electrochemical stripping,
Ion insertion, liquid phase ultrasound etc. [Acc. Chem. Res. 2014, 47, 1067-1075; Materials Letters.
2014, 121, 31-35; Small. 2015, 11, 605-612; Science, 2013,340,1226419.], so far
There is the problems such as yield is relatively low, intercalation degree hardly possible controls, stripping process is not green in these modern stripping means majorities, constrain two sulphur
Change the extensive use of molybdenum base nano material.
Patent（A kind of 201210512991.2 nanometer MOS 2 particle and preparation method and application）Using ionic liquid
Body or organic solvent are medium, and then ultrasonic wave added handles to obtain nanometer MOS 2 particle again for first grinding.It is this to grind and surpass
The separated batch process of sound, exist and peel off the shortcomings of cycle is long, charge stripping efficiency is low, cost is high, while the pattern of products therefrom
It is whard to control, it is difficult to obtain high radius-thickness ratio, the molybdenum disulfide nano sheet structure of high-specific surface area.
The content of the invention
It is an object of the invention to provide one kind molybdenite preparation widow is peeled off using sand milling and ultrasonic coupling effect are extensive
The method of layer molybdenum disulfide nano sheet.
To achieve the above object, the present invention uses following technical scheme：
The method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound-sand milling coupling, comprises the following steps：1）By brightness molybdenum
Ore deposit micro mist, which is scattered in peel off in solvent, forms suspension；
2）Dispersant, stripping auxiliary agent are dissolved in step 1）Suspension in ultrasonic disperse；
3）Step 2）Continuous peel off obtains curing to suspension after ultrasonic disperse under ultrasound, sand milling coupling simultaneously
Molybdenum nanometer sheet.Now molybdenum disulfide nano sheet is dispersed in suspension, and the suspension after stripping can pass through further work-up
The molybdenum disulfide nano sheet of powdery is made.Last handling process is：Standing, centrifugal classification, washing, freeze-drying.During centrifugal classification
Centrifugal rotational speed is 1500-10000 rpm.
Stripping solvent is N- methyl pyrrole network alkanones, and dispersant is polyvinylpyrrolidone, and stripping auxiliary agent is NaOH or NaCl.
The granularity of molybdenite micro mist is 5-50 microns, and the content of molybdenum disulfide is more than 99.8%.
Step 1）The solid content of molybdenite micro mist is 10-60 g/L in suspension；Step 2）Middle dispersant（PVP repeats single
Body）Mol ratio with molybdenite micro mist is 0.1-1, and the mol ratio for peeling off auxiliary agent and molybdenite micro mist is 0-1.
Step 3）Middle ultrasonic power is 200-350 W, and the rotating speed of sand mill is 1500-2250 rpm, coupling
Time is 0.5-6 h.
It is contemplated that a kind of low cost of development, high efficiency, relatively green, controllable magnanimity prepare molybdenum disulfide nano sheet
Method.Used initiation material is the molybdenite micro mist that China's reserves are big, physical and chemical performance is abundant, application prospect is wide, designs " sand
Mill-ultrasound " coupling peel off new method peel off molybdenite micro mist prepare molybdenum disulfide nano sheet on a large scale, realize from natural minerals to
The green conversion of performance function material, has significant application value and economic benefit.
More field of force coupling stripping systems such as present invention design sand milling, ultrasound, using molybdenite as starting material, ultrasound is produced
Cavitation be sanded caused by shearing simultaneously coupling, realize efficiently peel off.The abrading-ball that high speed operating is sanded hits brightness molybdenum
Ore deposit micro mist, shear action make interlayer and layer edge curl and split, and produce defect；Meanwhile ultrasonic cavitation promotes liquid
Molecule, stripping auxiliary agent etc. enter interlayer at the defects of splitting, and molybdenite is successively peeled off, auxiliary agent and dispersant are peeled off in medium
It is molybdenum disulfide nano sheet fine dispersion caused by stripping.The present invention be sanded-ultrasonic coupling peel off molybdenite prepare curing
Molybdenum nanometer sheet obtains yield and can reach 21.6wt%, and gained widow's layer molybdenum disulfide nano sheet has in terms of electro-catalysis and electrochemical sensing
Important application.
Brief description of the drawings
Fig. 1 is the installation drawing of sand milling-ultrasonic coupling stripping system；
Fig. 2 is that sand milling-ultrasonic coupling peels off schematic diagram；
Fig. 3 is the digital photograph of the gained molybdenum disulfide nano sheet suspension of embodiment 1；
Fig. 4 is the transmission electron microscope photo of the gained molybdenum disulfide nano sheet of embodiment 1；
Fig. 5 is the atomic force microscopy of the gained molybdenum disulfide nano sheet of embodiment 1；
Fig. 6 is the stereoscan photograph of the gained molybdenum disulfide nano sheet of embodiment 1；
Fig. 7 is the X ray diffracting spectrum of the gained molybdenum disulfide nano sheet of embodiment 1；
Fig. 8 is the N of the gained molybdenum disulfide nano sheet of embodiment 12Adsorption-desorption isothermal；
Fig. 9 is the UV-Visible absorption of gained molybdenum disulfide nano sheet suspension under the different splitting time of embodiment 1
Spectrum；
Figure 10 is the stripping yield of gained molybdenum disulfide nano sheet under the different time of embodiment 1（It is left）With speed（The right）
Figure；
Figure 11 is the stripping yield figure of molybdenum disulfide nano sheet obtained by 2 different splitting times of embodiment；
Figure 12 is the stripping yield and rate diagram of gained molybdenum disulfide nano sheet under the different time of embodiment 3；
Figure 13 be the initial molybdenite solid content of embodiment 4 be 35 g/L, molybdenum disulfide nano sheet obtained by different splitting times
The uv-visible absorption spectroscopy of suspension；
Figure 14 is different initial stripping yields and detachment rate of the molybdenite solid content in different splitting times of embodiment 4
Figure；
Figure 15 is that the ultraviolet-visible light that the ultrasonic power of embodiment 5 is gained molybdenum disulfide nano sheet suspension under 320 W is inhaled
Receive spectrum；
Figure 16 is the stripping yield and detachment rate figure of gained molybdenum disulfide nano sheet under the different ultrasonic power of embodiment 5；
Figure 17 be the sand mill rotating speed of embodiment 6 be under 1800 rpm gained molybdenum disulfide nano sheet suspension it is ultraviolet-can
See optical absorption spectra；
Figure 18 is the stripping yield and detachment rate of gained molybdenum disulfide nano sheet under the different sand mill rotating speeds of embodiment 6
Figure；
Figure 19 is the PVP monomers of embodiment 7 and MoS2Mol ratio be 1 when gained molybdenum disulfide nano sheet suspension it is ultraviolet-
Visible absorption spectrum；
Figure 20 is the stripping yield and detachment rate figure of gained molybdenum disulfide nano sheet under the different PVP contents of embodiment 7；
Figure 21 is the single field of force of effect experiment one（It is left：Individually ultrasound；It is right：Ultrasound is sanded substep and peeled off）The lower difference of effect
The uv-visible absorption spectroscopy of molybdenum disulfide nano sheet suspension obtained by splitting time；
Figure 22 is the single field of force of effect experiment one（I.e. individually ultrasound and ultrasound sand milling substep are peeled off）Coupled with more field of forces
（That is ultrasound-sand milling）The stripping yield and detachment rate figure of the lower molybdenum disulfide nano sheet of effect；
Figure 23 is the chemical property figure that gained molybdenum disulfide nano sheet is peeled off in ultrasound-sand milling coupling.
Embodiment
To realize a kind of device of the present invention, other have similar sand milling-ultrasound couple device disclosed in following examples
The device of function can be applied equally to the present invention.
Embodiment 1
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound-sand milling coupling, and step is as follows：
11.25 g molybdenite micro mists are scattered in 250 mL NMP（1-METHYLPYRROLIDONE, C5H9NO）Middle formed suspends
Liquid；2）3.9 g PVP are added therewith（Polyvinylpyrrolidone, (C6H9NO)n）, 20 min of ultrasound make its fully dispersed；3）Afterwards
It is transferred into sand mill（The rpm of rotating speed 2250）Reaction cavity, then acted in high-energy ultrasonic（Ultrasonic power is 280 W）Under, sand
Mill-ultrasonic coupling peels off 6 h；4）The molybdenum disulfide nano sheet suspension peeled off is stood into 24 h or so, centrifugal classification, classification
Centrifugal rotational speed is respectively 1500 rpm, 8000 rpm, 10000 rpm, and centrifugation time is respectively 45 min.Will 1500 rpm from
The molybdenum disulfide nano sheet solid content of upper strata suspension after the min of the heart 45 peels off the evaluation criterion of yield as evaluation：Using purple
The relative concentration of molybdenum disulfide nano sheet in outside-visible absorption spectra the real time measure suspension, and hanged using measuring is filtered
The absolute concentration of solid phase molybdenum disulfide nano sheet in supernatant liquid, working curve is made, unit of account time molybdenum disulfide nano sheet
Yield is peeled off, so as to calculate detachment rate.Finally can be further by the distillation water washing number of the sediment obtained by centrifugal classification
It is secondary, it is freeze-dried and produces few layer molybdenum disulfide nano sheet.
In the embodiment, mol ratio:PVP（Repeat unit）/MoS2=0.5。
Fig. 1 is the installation drawing of sand milling-ultrasonic coupling stripping system, i.e., using ultrasonic cell disintegration machine and sand mill phase mutual coupling
The method of conjunction, sand mill used configure ceramic-lined and cooling water system, a diameter of 2-5 mm of abrading-ball, ultrasonic probe are placed in
In the cavity of sand mill, ultrasonic cavitation is introduced simultaneously shear action is sanded, improves the charge stripping efficiency of molybdenite.
Fig. 2 is that sand milling-ultrasonic coupling peels off schematic diagram.The abrading-ball to run at high speed in sand mill hits molybdenite particulate,
Make its interlayer and layer edge cracks or defect, promote solvent molecule, stripping auxiliary agent etc. to enter layer under ultrasonic cavitation
Between, realize the efficient stripping of molybdenite.
Fig. 3 is the digital photograph of gained molybdenum disulfide nano sheet suspension after peeling off, and by the standing of 42 days, bottom did not had
Precipitation, darkly green suspension, can keep stable for a long time.
Fig. 4 is the transmission electricity of gained molybdenum disulfide nano sheet suspension products therefrom after 10000 rpm centrifuge 45 min
Sub- microphotograph.Good single crystal forms are presented in molybdenum disulfide nano sheet obtained by stripping, and lamella is relatively thin.
Fig. 5 is the AFM Analysis result of gained molybdenum disulfide nano sheet；It can be seen that resulting MoS2Nanometer
The thickness of piece is 1 nm or so, is individual layer.
Fig. 6 is that scanning electron of the gained molybdenum disulfide nano sheet suspension through 8000 rpm, 45 min products therefroms of centrifugation shows
Micro mirror photo, it can be seen that molybdenum disulfide nano sheet forms thin and translucent film due to being stacked with.
Fig. 7 is the XRD spectrum that gained molybdenum disulfide nano sheet suspension centrifuges 45 min products therefroms through 10000 rpm,
Its thing is mutually 2H-MoS2,（002）Crystallographic plane diffraction peak has widthization phenomenon, illustrates the thickness very little of molybdenum disulfide nano sheet.
Fig. 8 is gained molybdenum disulfide nano sheet N2Adsorption-desorption isothermal, centrifuge through 10000 rpm and produced obtained by 45 min
The BET surface area of thing is up to 926 m2 /g。
Fig. 9 is the uv-visible absorption spectroscopy of gained molybdenum disulfide nano sheet under different splitting times.Find out from figure,
With the extension of splitting time, the absorbance of the ultraviolet-visible absorption spectroscopy of centrifuged suspension at 660 nm gradually increases, root
According to Beer law, illustrate with the extension of time, the amount for peeling off gained molybdenum disulfide nano sheet steps up.
Figure 10 is that molybdenum disulfide nano sheet peels off yield and detachment rate figure, it can be seen that increases over time, stripping
Yield is increasing, and speed variation tendency is little.
Embodiment 2
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound-sand milling coupling, and step is as follows：
11.25 g molybdenite micro mists are scattered in 250 mL ethanol solutions（48%wt ethanol, C2H5OH）Middle formation suspension；
2）3.9 g PVP are added therewith（Polyvinylpyrrolidone, (C6H9NO)n）, 20 min of ultrasound make its fully dispersed；3）Turn afterwards
Move up into sand mill（The rpm of rotating speed 2250）Reaction cavity, then in ultrasonication（Ultrasonic power is 280 W）Under intercouple
Carry out peeling off 4 h；4）The suspension peeled off is stood into 2 h or so, centrifugal classification, respectively 1500 rpm, 5000 rpm,
45 min are centrifuged under 8000 rpm.Subsequent treatment is the same as embodiment 1.
Figure 11 is that molybdenum disulfide nano sheet peels off yield and detachment rate figure, with the extension of time, it is gradual to peel off yield
Increase, using ethanol solution as solvent, peel off yield and the linear change of splitting time.
Embodiment 3
Preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound-sand milling coupling, and step is as follows：
6.25 g molybdenite micro mists are scattered in 250 mL NMP（1-METHYLPYRROLIDONE, C5H9NO）Middle formation suspension；
2）2.17 g PVP are added therewith（Polyvinylpyrrolidone, (C6H9NO)n）, 20 min of ultrasound make its fully dispersed, add simultaneously
Salt (0.57gNaCl) or alkali (0.39gNaOH) peel off auxiliary agent；3）Sand mill is transferred into afterwards（The rpm of rotating speed 2250）Reaction chamber
Body, then in ultrasonication（Ultrasonic power is 280 W）Under intercouple carry out peel off 4 h；4）The suspension peeled off is quiet
24 h or so are put, centrifugal classification, centrifuge 45 min under 1500 rpm, 8000 rpm, 10000 rpm respectively.Subsequent treatment is same
Embodiment 1.
Figure 12 is that molybdenum disulfide nano sheet peels off yield and rate analysis figure, NMP to peel off solvent, add salt (NaCl) and
Alkali (NaOH) peels off influence of the auxiliary agent to stripping yield and efficiency.Both of which is added as can be seen from Fig. to charge stripping efficiency and yield
Increase, and add NaOH and improved more compared to NaCl, yield reaches 28.24%.
Embodiment 4
Influence of the different original solids contents to stripping yield and efficiency
Experimentation is the same as embodiment 1.
The initial content for changing molybdenite micro mist in the embodiment is respectively 3.75,6.25,8.75,11.25,13.75 g,
Corresponding solid content is respectively 15,25,35,45,55 g/L.
Figure 13 be original solids content be under 35 g/L, different time gained molybdenum disulfide nano sheet suspension it is ultraviolet-can
See spectrum；Find out from figure, with the extension of splitting time, the suction of the ultraviolet-visible absorption spectroscopy of centrifuged suspension at 660 nm
Luminosity gradually increases, and according to Beer law, splitting time is longer, and charge stripping efficiency is higher.
Figure 14 be peeled off under different initial molybdenite solid contents obtained by molybdenum disulfide nano sheet suspension in different strippings
Gained molybdenum disulfide nano sheet obtains solid content and peels off yield rate diagram in time.Found out by figure, with the increasing of original solids content
Add, detachment rate and yield have rising；When solid content is 15 g/L, the efficiency of stripping is maximum；With original solids content
Increase, in 45 g/L and 55 g/L, stripping yield is more or less the same.
Embodiment 5
Influence of the different ultrasonic powers to stripping yield and efficiency
Experimentation is the same as embodiment 1.
The embodiment only changes step 3 ultrasonic power of embodiment 1, ultrasonic power used in stripping is respectively with embodiment 1
200、240、280、320、350 W；
Figure 15 be when ultrasonic power is 320 W, molybdenum disulfide nano sheet suspension obtained by different splitting times it is ultraviolet-
Visible absorption spectra；Find out from figure, with the extension of splitting time, the ultraviolet-visible absorption spectroscopy of centrifuged suspension is in 660 nm
The absorbance at place gradually increases, and illustrates that charge stripping efficiency gradually steps up.
Figure 16 is under different ultrasonic power, the solid content of molybdenum disulfide nano sheet suspension obtained by under different splitting times
And peel off yield, rate diagram.As ultrasound peels off the increase of power, stripping yield first increases to be reduced afterwards, is reached most in 280 W
Greatly.
Embodiment 6
Influence of the different sand mill rotating speeds to stripping yield and efficiency
The experimentation of the embodiment only changes the rotating speed of sand mill with embodiment 1, and respectively 1500,1800,2250
rpm。
Figure 17 be sand mill rotating speed be 1800 rpm, the purple of molybdenum disulfide nano sheet suspension obtained by different splitting times
Outside-visible absorption spectra.Find out from figure, with the extension of splitting time, charge stripping efficiency gradually steps up.
Figure 18 is that gained molybdenum disulfide nano sheet suspension is peeled off under sand mill different rotating speeds in different splitting times
Solid content and stripping yield, rate diagram.As can be seen that gained molybdenum disulfide nano sheet yield under three different rotating speeds of sand mill,
Detachment rate is more or less the same.
Embodiment 7
Influence of the different PVP contents to stripping yield and efficiency
The experimentation of the embodiment only changes mol ratio with embodiment 1：PVP/MoS2=0、0.25、0.5、1。
Figure 19 is PVP/MoS2When=1 under different splitting times gained molybdenum disulfide nano sheet suspension ultraviolet-visible
Absorption spectrum.Find out from figure, splitting time is longer, and the absorbance of uv-visible absorption spectra of the suspension at 660 nm is got over
Greatly, according to Beer law, illustrate that splitting time is longer, it is higher to peel off yield.
Figure 20 is to peel off gained molybdenum disulfide nano sheet suspension consolidating in different splitting times under different PVP contents to contain
Amount and stripping yield, rate diagram.With the increase of PVP contents, the yield and speed of stripping increase.
Effect test one
Individually ultrasound, ultrasound, which are sanded to peel off step by step, couples stripping contrast with " ultrasound-sand milling "：
（1）Individually ultrasound is peeled off：11.25 g molybdenite micro mists are scattered in 250 mL NMP and form suspension, therewith
3.9 g PVP are added, 20 min of ultrasound make its fully dispersed, are placed in ultrasound stripping in wide-mouth bottle afterwards, and power is 280 W, when
Between be 4 h, peel off post-treatment condition with embodiment 1.
（2）Ultrasound is sanded substep and peeled off：11.25 g molybdenite micro mists are scattered in 250 mL NMP and form suspension,
Add 3.9 g PVP therewith, 20 min of ultrasound make fully dispersed, are placed in be sanded in chamber afterwards and carry out sand milling stripping, sand mill turns
Speed is 2250 rpm, and the time is 4 h, peels off post-treatment condition with embodiment 1.
（3）Ultrasound-sand milling coupling is peeled off：Coupling splitting time is 4 h, and other are the same as embodiment 1.
Figure 21（It is left：Individually ultrasound；It is right：Ultrasound, substep stripping is sanded）Substep is sanded and peels off for individually ultrasound, ultrasound
The uv-visible absorption spectra of molybdenum disulfide nano sheet obtained by different time.With the extension of splitting time, absorbance gradually increases
Add, illustrate that peeling off yield gradually steps up by Beer law.
Figure 22 is individually ultrasound, ultrasound sand milling substep is peeled off and gained under three kinds of modes such as stripping is coupled with " ultrasound-sand milling "
Stripping yield, rate diagram of the molybdenum disulfide nano sheet suspension in different splitting times.It can be seen that three kinds of different strippings
Under mode, coupling release effect can give full play to the synergy of the shock shear action of sand milling and the cavitation of ultrasound, from
And improve and peel off yield.
Effect test two
The stripping process of molybdenum disulfide nano sheet is the same as implementation 1；The chemical property of test gained molybdenum disulfide nano sheet.Will
Ultrasound-sand milling coupling is peeled off suspension and centrifuged in 8000-10000 rpm sections, and few layer MoS is made2Nanometer sheet.Take 4 mg
Gained widow's layer MoS2Nanometer sheet is scattered in 950 ml DMF (N-N dimethylformamides) and 50 ml and draws in luxuriant and rich with fragrance solution simultaneously ultrasonic point
Dissipate, then take 4 ml to make working electrode coated on glass-carbon electrode.Then using saturated calomel electrode as reference electrode, platinum electricity
Extremely to electrode, electrochemical property test is carried out.The sweep speed of the Linear Circulation volt-ampere of electrocatalytic hydrogen evolution performance is 2 mV/s.
Figure 23 is gained widow's layer MoS2The electrocatalysis characteristic of nanometer sheet.Found out by figure, the few layer MoS of high rotating speed centrifugation gained2Receive
Rice piece centrifuges gained sample than molybdenite micro mist and the slow-speed of revolution, has smaller OCP and bigger current density, and
Smaller Ta Feier slopes.High rotating speed centrifugation gained MoS2Nanometer sheet sample is thinner, and surface-active site is increased, and is more beneficial for
Liberation of hydrogen catalytic reaction.
Claims (2)
1. the method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound-sand milling coupling, it is characterised in that including following step
Suddenly：1）Molybdenite micro mist is scattered in peel off in solvent and forms suspension；
2）Dispersant, stripping auxiliary agent are dissolved in step 1）Suspension in ultrasonic disperse；
3）Step 2）The suspension continuous stripping under ultrasound, sand milling coupling simultaneously after ultrasonic disperse obtains molybdenum disulfide and received
Rice piece；
Wherein, it be N- methyl pyrrole network alkanones to peel off solvent, and dispersant is polyvinylpyrrolidone, peel off auxiliary agent for NaOH or
NaCl；Step 1）The solid content of molybdenite micro mist is 10-60 g/L in suspension；Step 2）Middle dispersant and molybdenite micro mist
Mol ratio is 0.1-1, and the mol ratio for peeling off auxiliary agent and molybdenite micro mist is 0-1；Step 3）Middle ultrasonic power is 200-350
W, rotating speed during sand milling is 1500-2250 rpm, and the time of coupling is 0.5-6 h.
2. the method that preparing molybdenum disulfide from molybdenite nanometer sheet is peeled off in ultrasound as claimed in claim 1-sand milling coupling, its feature
It is, the granularity of molybdenite micro mist is 5-50 microns, and the content of molybdenum disulfide is more than 99.8%.
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