CN107365259A - Molybdenum disulfide dispersant, molybdenum disulfide dispersion, its preparation method and application - Google Patents

Molybdenum disulfide dispersant, molybdenum disulfide dispersion, its preparation method and application Download PDF

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CN107365259A
CN107365259A CN201610310516.5A CN201610310516A CN107365259A CN 107365259 A CN107365259 A CN 107365259A CN 201610310516 A CN201610310516 A CN 201610310516A CN 107365259 A CN107365259 A CN 107365259A
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oligomer
phenylamine
molybdenum disulfide
derivative
aniline
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CN107365259B (en
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***
陈佳
陈诚
赵海超
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Priority to CN201610310516.5A priority Critical patent/CN107365259B/en
Priority to PCT/CN2016/101469 priority patent/WO2017193532A1/en
Priority to US16/300,273 priority patent/US10843153B2/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C211/00Compounds containing amino groups bound to a carbon skeleton
    • C07C211/43Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
    • C07C211/54Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton having amino groups bound to two or three six-membered aromatic rings
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • C01G39/06Sulfides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C233/00Carboxylic acid amides
    • C07C233/01Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
    • C07C233/34Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups
    • C07C233/42Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by a carbon atom of a six-membered aromatic ring
    • C07C233/43Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by a carbon atom of a six-membered aromatic ring having the carbon atom of the carboxamide group bound to a hydrogen atom or to a carbon atom of a saturated carbon skeleton
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer

Abstract

The invention discloses a kind of molybdenum disulfide (MoS2) dispersant, molybdenum disulfide dispersion, its preparation method and application.The molybdenum disulfide dispersant includes that the oligomer of phenylamine and/or oligomer of phenylamine derivative to make molybdenum disulfide be stably dispersed in the decentralized media such as Conventional solvents can be combined with molybdenum disulfide by physical action.The present invention is used as molybdenum disulfide dispersant by the use of the cheap oligomer of phenylamine of cost and/or its derivative, and the dispersant is simply mixed in decentralized medium with molybdenum disulfide, pass through Physical interaction between the two, molybdenum disulfide two-dimensional nano piece is obtained using simple liquid phase stripping means, its physical arrangement and chemical property without detriment to molybdenum disulfide, operating process is simple, implement beneficial to extensive, and the molybdenum disulfide two-dimensional nano tablet quality peeled off is high, is had broad application prospects in fields such as semiconductor, the energy, wear proof lubricating painting materials, composites.

Description

Molybdenum disulfide dispersant, molybdenum disulfide dispersion, its preparation method and application
Technical field
Molybdenum disulfide dispersion and redispersible is prepared the present invention is more particularly directed to a kind of molybdenum disulfide dispersant, by physical method The method of molybdenum disulfide powder.
Background technology
Molybdenum disulfide is a kind of layered semiconductor material, many in lubrication, ion exchange, absorption, conduction, separation and catalysis etc. Field has broad application prospects.But it is to be combined with weaker Van der Waals force between molybdenum disulfide category lamella, under the influence of the external world, Easily curl and reunite, cause scattered limited in Conventional solvents, this just largely limits its application.To obtain two The two-dimension nano materials of molybdenum sulfide, industry propose all multi-schemes.For example, there is researcher to pass through in the mixing containing oxidant Stir or be ultrasonically treated in solvent, molybdenum disulfide can in organic solvent be peeled off and form molybdenum disulfide nano sheet.For example, also have Researcher water bath sonicator 0.5~2 hour, obtains mixed solution by the way that amphiphilic surfactant is dissolved in organic solvent; Then molybdenum disulfide powder is added in mixed solution, ultrasound, centrifugation, removes supernatant, collect precipitation, dry, obtain Solids, that is, the two-dimensional layer nano material after peeling off.In another example there is researcher to pass through in MoS2Intercalation reaction lithium, and lead to Crossing ultrasound realizes MoS2Stable dispersion of the lamella in water, but the process is complicated and limits its application.For another example grind Study carefully personnel and report the achievable MoS in the ethanol and water mixed solvent necessarily matched2Stripping, but dispersion concentration is very low, only For 0.018mg/mL.Also researcher is acted on by the assisted milling of 1-METHYLPYRROLIDONE and sonication, is ground by changing Time consuming and grinding-sonication time realize the stable dispersion of molybdenum disulfide in aqueous.But foregoing existing curing Molybdenum two-dimensional nano piece preparation method generally existing operation difficulty is big, it is difficult to the defects of scale is implemented, and obtained molybdenum disulfide two Wiener rice flake products quality is unstable.
The content of the invention
It is a primary object of the present invention to provide a kind of molybdenum disulfide dispersant, molybdenum disulfide dispersion, its preparation method and application, To overcome deficiency of the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiments of the invention provide a kind of molybdenum disulfide dispersant, and it includes oligomer of phenylamine and/or oligomer of phenylamine derivative, And the oligomer of phenylamine and/or oligomer of phenylamine derivative can be combined to make molybdenum disulfide by physical action with molybdenum disulfide It is stably dispersed in decentralized medium.
Further, oligomer of phenylamine and/or the oligomer of phenylamine derivative includes aniline tripolymer, Tetraaniline, aniline Any one or any one derivative in pentamer and the aggressiveness of aniline six.
The embodiment of the present invention additionally provides the compound of a kind of molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative (also It is regarded as the molybdenum disulfide of oligomer of phenylamine and/or oligomer of phenylamine Derivatives Modified), the oligomer of phenylamine and/or aniline are low Polymers derivative includes any one in aniline tripolymer, Tetraaniline, aniline pentamer and the aggressiveness of aniline six or any one The derivative of kind.
The embodiment of the present invention additionally provides a kind of oligomer of phenylamine and/or oligomer of phenylamine derivative as molybdenum disulfide dispersant Purposes, oligomer of phenylamine and/or the oligomer of phenylamine derivative include aniline tripolymer, Tetraaniline, aniline pentamer and Any one or any one derivative in the aggressiveness of aniline six.
The embodiment of the present invention additionally provides a kind of liquid phase and peels off the method for preparing two-dimentional molybdenum disulfide nano material, and it includes:By benzene Amine oligomer and/or oligomer of phenylamine derivative are sufficiently mixed with molybdenum disulfide powder in the decentralized medium such as water and/or organic solvent, Form the stable dispersions of two-dimentional molybdenum disulfide nano material.
The embodiment of the present invention additionally provides a kind of molybdenum disulfide dispersion, and it is included:Decentralized medium;And it is scattered in described point In dispersion media, foregoing any compound.
The embodiment of the present invention additionally provides a kind of preparation method of molybdenum disulfide dispersion, and it includes:By molybdenum disulfide and the benzene Amine oligomer and/or oligomer of phenylamine derivative are uniformly mixed to form stabilising dispersions in decentralized medium.
The embodiment of the present invention additionally provides a kind of redispersible molybdenum disulfide powder, and it is by removing foregoing any two Decentralized medium in molybdenum sulfide dispersion and the powder obtained, and the powder can be directly scattered in the decentralized medium again In.
Realize that molybdenum disulfide is scattered with redisperse method based on physical method the embodiments of the invention provide one kind, it includes:
By molybdenum disulfide and foregoing any oligomer of phenylamine and/or oligomer of phenylamine derivative in decentralized medium uniformly It is mixed to form stabilising dispersions,
Remove the decentralized medium in the dispersion and obtain molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative Compound,
And be scattered in the compound in decentralized medium again, stabilising dispersions are formed again.
Further, the molybdenum disulfide is two-dimentional molybdenum disulfide nano material.
Further, the decentralized medium may be selected from but be not limited to water, in organic solvent, macromolecule resin any one or two The combination of the kind above.
Compared with prior art, beneficial effects of the present invention include:Using be readily synthesized, the oligomer of phenylamine that cost is cheap and/or Its derivative is as molybdenum disulfide dispersant, and by the dispersant and molybdenum disulfide at decentralized medium (such as water, organic solvent etc.) In be simply mixed, pass through Physical interaction between the two, you can be substantially improved molybdenum disulfide, particularly molybdenum disulfide two dimension Decentralization and dispersion stabilization of the nano material in decentralized medium;Moreover, nationality is by the oligomer of phenylamine and/or oligomer of phenylamine Derivative can also obtain molybdenum disulfide two-dimensional nano piece, its physics without detriment to molybdenum disulfide by simple liquid phase stripping means Structure and chemical property, process cleans are efficient and easy to operate, implement beneficial to scale, and the molybdenum disulfide two-dimensional nano peeled off Piece has broad application prospects in fields such as semiconductor, the energy, wear proof lubricating painting materials, composites.
Brief description of the drawings
Fig. 1 be in the embodiment of the present invention 1 molybdenum disulfide without dispersant and have dispersant effect under disperse photo;
Fig. 2 is the molybdenum disulfide nano sheet SEM photograph after being peeled off in the embodiment of the present invention 1.
Embodiment
As it was previously stated, molybdenum disulfide two-dimensional nano piece is easily sent out because piece interlayer has strong interaction in usual vehicle Raw precipitation (referring to Fig. 1) of reuniting, for inventor through studying for a long period of time and largely putting into practice, spy proposes technical scheme, And obtain unexpected good technique effect.It will explain as follows the progress such as technical scheme and its effect is detailed State.
The one side of the embodiment of the present invention provides a kind of molybdenum disulfide dispersant, and it includes oligomer of phenylamine and/or aniline is oligomeric Thing derivative, and the oligomer of phenylamine and/or oligomer of phenylamine derivative can be combined to make by physical action with molybdenum disulfide Molybdenum disulfide is stably dispersed in decentralized medium.
Further, the molybdenum disulfide dispersant is selected from oligomer of phenylamine and/or oligomer of phenylamine derivative with aromatic structure Thing.
Further, in the case where any additive and reactant need not be added, simple physical mixed (such as machine is only passed through The physics modes such as tool stirring, ultrasound, vibration, can also coordinate other suitable non-physical methods in some embodiments certainly), And using the physics weak interaction between the dispersant and molybdenum disulfide, with regard to can make molybdenum disulfide decentralized medium (such as water, The Conventional solvents such as organic solvent) in realize stable dispersion.
Further, oligomer of phenylamine and/or the oligomer of phenylamine derivative includes aniline tripolymer, Tetraaniline, aniline Any one or any one derivative in pentamer and the aggressiveness of aniline six.
Preferably, the oligomer of phenylamine derivative includes the micromolecular compound containing oligomer of phenylamine, particularly carboxy blocking Oligomer of phenylamine derivative, alkyl-substituted oligomer of phenylamine derivative etc..Such as the aniline tripolymer of carboxy blocking, the tetramer, Pentamer, or chain alkyl or alkoxy end-capped aniline tripolymer, the tetramer or pentamer etc..
Preferably, the oligomer of phenylamine derivative may be selected from the polymer containing oligomer of phenylamine grafting or block.Such as poly- second two Alcohol end-blocking oligomer of phenylamine (the aniline tripolymer of polyethylene glycol end-blocking, the tetramer and pentamer etc.);PLA end-blocking aniline is oligomeric Thing (aniline tripolymer, the tetramer and pentamer of PLA end-blocking etc.).
More specifically, the oligomer of phenylamine derivative is preferably from the compound with following any chemical formula:
Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic.
Further, if not special instruction, the then oligomer of phenylamine and/or oligomer of phenylamine derivative addressed in this manual are equal It may be selected from foregoing all kinds of oligomer of phenylamine and/or oligomer of phenylamine derivatives.
Further, oligomer of phenylamine and/or the oligomer of phenylamine derivative can be combined by physical action with molybdenum disulfide, So that Maximum single layer distribution threshold value of the molybdenum disulfide in decentralized medium (such as water, organic solvent etc.) reaches 10mg/mL.Need Bright, " Maximum single layer distribution threshold value " described herein corresponds to the situation of the molybdenum disulfide dispersant using minimal effective dose.
Suitable for the present invention oligomer of phenylamine derivative can commercially available from approach obtain, can also bibliography (for example, J.Amer.Chem.Soc.,1986,108,8311;Macromol.Rapid Commun.,2011,32,35;CN 104016876A; CN1887854A etc.) self-control.
Further, the molybdenum disulfide is two-dimentional molybdenum disulfide nano material, and preferably thickness is 1~20nm molybdenum disulfide Two-dimensional nano piece.
Further, the decentralized medium includes Conventional solvents, such as water or organic solvent etc. or macromolecule resin etc.. For instance, it may be preferable to from alkaline aqueous solution etc. (alkali therein can be NaOH, KOH etc.).For example, the organic solvent can Selected from low boiling point solvent and/or high boiling point polar organic solvent, for example, preferably from ethanol, tetrahydrofuran, dimethylformamide, Any one in dimethyl sulfoxide (DMSO), chloroform and 1-METHYLPYRROLIDONE or two or more combinations.For example, the high score subtree Fat can be polyethylene glycol, polypropylene glycol etc..
Further, if not special instruction, the then decentralized medium addressed in this manual may be selected from foregoing water, all kinds of have Solvent or macromolecule resin etc..
The one side of the embodiment of the present invention additionally provides molybdenum disulfide and the oligomer of phenylamine and/or oligomer of phenylamine derivative Compound.
More preferable, the weight ratio of oligomer of phenylamine and/or the oligomer of phenylamine derivative and molybdenum disulfide is 0.1~10:1, Especially preferably 0.2~2:1.
Further, the molybdenum disulfide is two-dimentional molybdenum disulfide nano material, and preferably thickness is 1~20nm molybdenum disulfide Two-dimensional nano piece.
The one side of the embodiment of the present invention additionally provides a kind of oligomer of phenylamine and/or oligomer of phenylamine derivative as curing The purposes of molybdenum dispersant.
Further, the molybdenum disulfide is two-dimentional molybdenum disulfide nano material, and preferably thickness is 1~20nm molybdenum disulfide Two-dimensional nano piece.
The one side of the embodiment of the present invention additionally provides a kind of liquid phase and peels off the method for preparing two-dimentional molybdenum disulfide nano material, its Including:By oligomer of phenylamine and/or oligomer of phenylamine derivative with molybdenum disulfide powder at decentralized medium (such as water and/or organic solvent) In be sufficiently mixed (such as by the physics modes such as mechanical agitation, ultrasound mix), form the stabilization of two-dimentional molybdenum disulfide nano material Dispersion liquid.
More preferable, methods described includes:By oligomer of phenylamine and/or oligomer of phenylamine derivative with molybdenum disulfide powder in water And/or the stable dispersions of two-dimentional molybdenum disulfide nano material are thoroughly mixed to form in organic solvent, afterwards to the stable dispersions Centrifugal treating is carried out, collects and obtains the compound of two-dimentional molybdenum disulfide nano material and oligomer of phenylamine and/or oligomer of phenylamine derivative Thing.
More preferable, methods described includes:By oligomer of phenylamine and/or oligomer of phenylamine derivative, alkali (such as NaOH, KOH etc.) stable dispersions of two-dimentional molybdenum disulfide nano material are thoroughly mixed to form in water with molybdenum disulfide powder, it is right afterwards The stable dispersions carry out centrifugal treating, collect the two-dimentional molybdenum disulfide nano material of acquisition and oligomer of phenylamine and/or aniline are oligomeric The compound of thing derivative.
More preferable, methods described includes:Make aniline low from least one of physics modes such as ultrasound, stirring, vibration Polymers and/or oligomer of phenylamine derivative are sufficiently mixed with molybdenum disulfide powder in water and/or organic solvent.
Further, the two-dimentional molybdenum disulfide nano material is the molybdenum disulfide two-dimensional nano piece that thickness is 1~20nm.
The liquid phase of the present invention peels off the method for molybdenum disulfide by oligomer of phenylamine and/or oligomer of phenylamine derivative and molybdenum disulfide Between Physical interaction, it is possible to achieve stripping of the molybdenum disulfide in the decentralized medium such as water and/or organic solvent and good point Dissipate, whole stripping process clean and effective and simple to operate, not need harshness reaction condition (such as high temperature, high pressure, strong acid and The reaction conditions such as highly basic), beneficial to large-scale production and the application for carrying out product downstream, the wiener of molybdenum disulfide two particularly peeled off Rice piece is expected to have broad application prospects in fields such as semiconductor, the energy, wear proof lubricating painting materials, composites.
The one side of the embodiment of the present invention additionally provides a kind of molybdenum disulfide dispersion, and it is included:Decentralized medium;And point Dissipate in the decentralized medium, foregoing any compound.
Further, the molybdenum disulfide dispersion is flow-like dispersion, preferably liquid dispersion or slurry.
Preferably, the molybdenum disulfide that the molybdenum disulfide dispersion includes may be up to 10mg/mL, and especially preferably 0.1mg/mL~ 10mg/mL, more preferably 0.1mg/mL~2.5mg/mL.
The one side of the embodiment of the present invention additionally provides the preparation method of a kind of molybdenum disulfide dispersion, and it includes:By curing Molybdenum and oligomer of phenylamine and/or oligomer of phenylamine derivative are uniformly mixed to form stabilising dispersions in decentralized medium.
Further, the weight ratio preferably 0.1~10 of oligomer of phenylamine and/or the oligomer of phenylamine derivative and molybdenum disulfide:1, Especially preferably 0.2~2:1.
Further, the molybdenum disulfide is preferably two-dimentional molybdenum disulfide nano material, and especially preferably thickness is 1~20nm's Molybdenum disulfide two-dimensional nano piece.
Further, the decentralized medium includes any one in water, organic solvent, macromolecule resin or two or more groups Close, preferably be selected from organic solvent, such as previously recited a variety of organic solvents.
Preferably, the molybdenum disulfide that the stabilising dispersions include may be up to 10mg/mL, especially preferably 0.1mg/mL~10 Mg/mL, more preferably 0.1mg/mL~2.5mg/mL.
The one side of the embodiment of the present invention additionally provides a kind of redispersible molybdenum disulfide powder, and it is by removing as previously described Any molybdenum disulfide dispersion in decentralized medium and the powder that obtains, and the powder can be directly scattered in institute again State in decentralized medium.
The one side of the embodiment of the present invention is additionally provided a kind of molybdenum disulfide realized based on physical method and disperseed and redisperse side Method, it includes:
Molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative are uniformly mixed to form stable dispersion in decentralized medium Body,
Remove the decentralized medium in the dispersion and obtain molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative Compound,
And be scattered in the compound in decentralized medium again, stabilising dispersions are formed again.
Further, the molybdenum disulfide is preferably two-dimentional molybdenum disulfide nano material, and especially preferably thickness is 1~20nm's Molybdenum disulfide two-dimensional nano piece.
Further, oligomer of phenylamine and/or the weight of oligomer of phenylamine derivative and molybdenum disulfide ratio are in the compound 0.1~10:1, preferably 0.2~2:1.
In some embodiments, methods described may also include:Molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine are derived Thing is uniformly mixed to form stable dispersions in water and/or organic solvent, and processing is dried (i.e. to the stable dispersions afterwards Remove water, organic solvent etc.) and form the compound in powder shaped.
Wherein, the mode of the drying process at least may be selected from any one in spray drying, rotary evaporation and vacuum drying, But not limited to this.
The molybdenum disulfide of the present invention is scattered and redisperse method is easy to operate, and cost is cheap, and beneficial to prepare with scale, that is obtained can The molybdenum disulfide composite powder of redisperse has broad application prospects in fields such as functional coating, heat conduction and composite enhancings.
The technical scheme in the embodiment of the present invention is described in detail below in conjunction with some embodiments and accompanying drawing.Obviously, institute The embodiment of description is only part of the embodiment of the present invention, and and not all embodiment.Based on the embodiment in the present invention, sheet The every other embodiment that field those of ordinary skill is obtained on the premise of creative work is not made, belongs to the present invention The scope of protection.
The synthesis of the aniline tripolymer of embodiment 1 and its stripping for molybdenum disulfide nano sheet
The synthesis of aniline tripolymer:P-phenylenediamine sulfate (8.87g), aniline (5.56g) are added to contain and fill hydrochloric acid solution (1 M, 500mL) three-neck flask in, be cooled to -5 DEG C.150mL ammonium persulfates (13.62g) hydrochloric acid (1M) solution is led to Cross dropping funel to be slowly added dropwise into above-mentioned reaction bulb, wait after being added dropwise, continue stirring reaction 1h, reaction product is taken out Filter, is cleaned with a large amount of deionized waters, obtains blackish green solid product.Then 10wt% ammonia spirit wash products are used, then Cleaned twice with deionized water, product is finally placed in dried for standby in 40 DEG C of vacuum drying chamber.Obtained aniline tripolymer is in second There is good dissolubility in alcohol, ethyl acetate, tetrahydrofuran, chloroform, dimethylformamide equal solvent.
The aniline tripolymer that the present embodiment obtains is mixed by a certain percentage with molybdenum disulfide powder, and is dissolved in ethanol (EtOH) respectively In tetrahydrofuran (THF), ultrasonic disperse 10 minutes, dispersion effect of the molybdenum disulfide under oligomer of phenylamine effect is examined, such as Shown in Tables 1 and 2, (the shape of the molybdenum disulfide nano sheet of stripping when molybdenum disulfide nano sheet concentration is in below 2.5mg/mL Looks see Fig. 2), aniline tripolymer-molybendum disulfide complexes can form stable dispersion liquid in ethanol and tetrahydrofuran, without bright Show precipitation;And stood when molybdenum disulfide nano sheet concentration reaches 5mg/mL 1 it is small when after the aggregations of partial plies can occur Precipitate (referring to Fig. 1).
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 1 under the effect of aniline tripolymer in ethanol:Aniline tripolymer=1:1)
5mg/10mL 15mg/10mL 25mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment Well, there is partly precipitated
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 2 under the effect of aniline tripolymer in tetrahydrofuran:Aniline tripolymer=1:1)
5mg/10mL 15mg/10mL 25mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment There is partly precipitated
The synthesis of the Tetraaniline of embodiment 2 and its stripping for molybdenum disulfide nano sheet
4-aminodiphenylamine (11.08g, 60mmol), acetone (300mL), salt are sequentially added in 500mL round-bottomed flask Sour (1M, 75mL) solution, deionized water (300mL), stirring is to being completely dissolved.Then by ammonium persulfate (13.6g, 60mmol) Hydrochloric acid solution (1M, 150mL) be gradually added drop-wise in above-mentioned solution, after being added dropwise, in -5 DEG C of lower reaction 3 hours, instead It should terminate, be filtered with Buchner funnel, be cleaned again with 10wt% ammoniacal liquor afterwards, then be cleaned twice with a large amount of deionized waters, Finally, it is placed on dried for standby in 40 DEG C of vacuum drying chamber.The Tetraaniline of acquisition tetrahydrofuran, ethyl acetate, nitrogen, There is good dissolubility in nitrogen-dimethylformamide.
The Tetraaniline of the present embodiment and molybdenum disulfide powder are dissolved in THF by a certain percentage, ultrasonic disperse 10 minutes, examined Its dispersion effect in a solvent, as shown in table 3, when molybdenum disulfide nano sheet concentration is in below 2.5mg/mL, aniline four Aggressiveness-molybendum disulfide complexes can form stable dispersions in tetrahydrofuran, and no obvious sediment occurs, and works as molybdenum disulfide nano sheet When concentration reaches 5mg/mL, then part aggregate and precipitate can occur.
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 3 under Tetraaniline effect in tetrahydrofuran:Tetraaniline=1:1)
5mg/10mL 15mg/10mL 25mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment There is partly precipitated
The synthesis of the carboxy blocking aniline tripolymer of embodiment 3 and its stripping for molybdenum disulfide nano sheet
Aniline tripolymer (2.92g) is dissolved in 50mL THF, then adds maleic anhydride (2.46g), reaction 3 is small at 40 DEG C When, reaction product petroleum ether precipitation, obtain carboxy blocking aniline tripolymer (4.8g).Weigh carboxylated aniline tripolymer and 2 The NaOH of times molar equivalent and (and the weight ratio of carboxylated aniline tripolymer is 1 with molybdenum disulfide nano sheet powder:1), configure The aqueous solution of various concentrations, ultrasonic disperse 10 minutes.Dispersion effect is as shown in table 1, when molybdenum disulfide nano sheet concentration is 2.5 Stable dispersion liquid can be formed during below mg/mL, for concentration in 5mg/mL, molybdenum disulfide nano sheet tends to saturation in water, There is partly precipitated to have partly precipitated after standing 1 hour.
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 4 under the effect of carboxy blocking aniline tripolymer in water:Carboxy blocking aniline trimerization Body=1:1)
5mg/10mL 15mg/10mL 25mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment There is partly precipitated
The synthesis of 4 carboxylic acid-terminated Tetraaniline of embodiment and its stripping for molybdenum disulfide nano sheet
Tetraaniline (2.1g) is added in 50mL THF, is then added maleic anhydride (0.68g), is reacted 3 hours at 40 DEG C, With petroleum ether precipitation, Tetraaniline carboxy derivatives are obtained.By obtained Tetraaniline carboxy derivatives and 2 times of molar equivalents NaOH and molybdenum disulfide powder be made into the certain density aqueous solution, ultrasound 10 minutes, dispersion effect is as shown in table 5, two sulphur Uniform dispersion can be formed in below 3mg/mL by changing molybdenum nanometer sheet concentration, and concentration is in 5mg/mL, molybdenum disulfide nano Piece tends to saturation in water, has partly precipitated to have partly precipitated after standing 1 hour.
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 5 under the effect of carboxylic acid-terminated Tetraaniline in water:Carboxylic acid-terminated aniline four Aggressiveness=1:1)
5mg/10mL 15mg/10mL 30mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment There is partly precipitated
The synthesis of the carboxy blocking aniline pentamer of embodiment 5 and its stripping for molybdenum disulfide nano sheet
Carboxy blocking aniline pentamer used in the present embodiment is by document synthesis (SCI, 2004,9,1768).It will be obtained The NaOH and molybdenum disulfide powder of aniline pentamer carboxy derivatives and 2 times of molar equivalents are configured to the certain density aqueous solution, Ultrasound 10 minutes, dispersion effect is as shown in table 6, can be formed when molybdenum disulfide nano sheet concentration is in below 2.5mg/mL Even dispersion liquid, for concentration in 5mg/mL, molybdenum disulfide nano sheet tends to saturation in water, has partly precipitated after standing 1 hour Occur.
Dispersion effect (molybdenum disulfide of the molybdenum disulfide of table 6 under the effect of carboxy blocking aniline pentamer in water:Carboxy blocking aniline five Aggressiveness=1:1)
5mg/10mL 15mg/10mL 25mg/10mL 50mg/10mL
Well, no obvious sediment Well, no obvious sediment Well, no obvious sediment There is partly precipitated
The stable molybdenum disulfide two-dimensional nano piece dispersion liquid that embodiment 1- embodiments 5 are obtained is formed by being dried in vacuo mode processing Powder (refers to Fig. 2), after these powders are scattered in foregoing Conventional solvents again, by be stirred vigorously or ultrasound, i.e., Can form the dispersion (such as refering to Fig. 1) of stable dispersion, the dispersion stand at room temperature more than 10 days and substantially without Sedimentation phenomenon occurs.
It should be noted that molybdenum disulfide dispersant used by example, decentralized medium, all kinds of raw materials and process conditions are performed as described above It is more typical example, but by the checking of inventor's lot of experiments, disperses in the other molybdenum disulfide of those listed above Agent, decentralized medium, raw material and process conditions etc. are also applicable, and also equal attainable cost invents claimed technique effect.
Postscript, herein, term " comprising ", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, So that process, method, article or equipment including a series of elements not only include those key elements, but also including not having The other element being expressly recited, or also include for this process, method, article or the intrinsic key element of equipment.
It should be appreciated that described above is only the embodiment of the present invention, it is noted that for the common skill of the art For art personnel, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (15)

  1. A kind of 1. molybdenum disulfide dispersant, it is characterised in that including oligomer of phenylamine and/or oligomer of phenylamine derivative, and the benzene Amine oligomer and/or oligomer of phenylamine derivative can be combined to make molybdenum disulfide stable dispersion by physical action with molybdenum disulfide In in decentralized medium.
  2. 2. molybdenum disulfide dispersant according to claim 1, it is characterised in that:The oligomer of phenylamine and/or aniline are oligomeric Thing derivative include aniline tripolymer, Tetraaniline, aniline pentamer and the aggressiveness of aniline six in any one or any one Derivative;Preferably, the oligomer of phenylamine derivative includes the micromolecular compound containing oligomer of phenylamine, particularly preferably certainly Polymer containing oligomer of phenylamine grafting or block, particularly preferably the oligomer of phenylamine derivative or oligomer of phenylamine from carboxy blocking Derivative, particularly preferably from the compound with following any chemical formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic;And/or the molybdenum disulfide is two-dimentional molybdenum disulfide nano material, Preferably thickness is 1~20nm molybdenum disulfide two-dimensional nano piece;And/or the decentralized medium includes water, organic solvent and height Any one in molecule resin or two or more combinations.
  3. 3. molybdenum disulfide and oligomer of phenylamine and/or the compound of oligomer of phenylamine derivative, the oligomer of phenylamine and/or aniline Oligomer derivative includes any one in aniline tripolymer, Tetraaniline, aniline pentamer and the aggressiveness of aniline six or any A kind of derivative;Preferably, the oligomer of phenylamine derivative includes the micromolecular compound containing oligomer of phenylamine, especially excellent Selected from the polymer containing oligomer of phenylamine grafting or block, particularly preferably taken from the oligomer of phenylamine derivative or alkyl of carboxy blocking The oligomer of phenylamine derivative in generation, particularly preferably from the compound with following any chemical formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic.
  4. 4. compound according to claim 3, it is characterised in that:Oligomer of phenylamine and/or the oligomer of phenylamine derivative Weight ratio with molybdenum disulfide is 0.1~10:1, preferably 0.2~2:1;And/or the molybdenum disulfide is two-dimentional molybdenum disulfide nano Material, preferably thickness are 1~20nm molybdenum disulfide two-dimensional nano piece.
  5. 5. the purposes of oligomer of phenylamine and/or oligomer of phenylamine derivative as molybdenum disulfide dispersant, the oligomer of phenylamine and/ Or oligomer of phenylamine derivative includes any one in aniline tripolymer, Tetraaniline, aniline pentamer and the aggressiveness of aniline six Or the derivative of any one;Preferably, the oligomer of phenylamine derivative includes the micromolecular compound containing oligomer of phenylamine, The particularly preferably polymer of the grafting of self-contained oligomer of phenylamine or block, particularly preferably from the oligomer of phenylamine derivative of carboxy blocking or Alkyl-substituted oligomer of phenylamine derivative, particularly preferably from the compound with following any chemical formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic.
  6. 6. purposes according to claim 5, it is characterised in that:The molybdenum disulfide is two-dimentional molybdenum disulfide nano material, Preferably thickness is 1~20nm molybdenum disulfide two-dimensional nano piece.
  7. 7. a kind of liquid phase peels off the method for preparing two-dimentional molybdenum disulfide nano material, it is characterised in that including:By oligomer of phenylamine and / or oligomer of phenylamine derivative be sufficiently mixed with molybdenum disulfide powder in water and/or organic solvent, form two-dimentional molybdenum disulfide nano The stable dispersions of material.
  8. 8. liquid phase according to claim 7 peels off the method for preparing two-dimentional molybdenum disulfide nano material, it is characterised in that including: Oligomer of phenylamine and/or oligomer of phenylamine derivative are thoroughly mixed to form two with molybdenum disulfide powder in water and/or organic solvent The stable dispersions of molybdenum disulfide nano material are tieed up, centrifugal treating is carried out to the stable dispersions afterwards, collects and obtains two dimension two Molybdenum sulfide nano material and oligomer of phenylamine and/or the compound of oligomer of phenylamine derivative.
  9. 9. the liquid phase according to claim 7 or 8 peels off the method for preparing two-dimentional molybdenum disulfide nano material, it is characterised in that Including:Make oligomer of phenylamine and/or oligomer of phenylamine derivative and two sulphur from least one of ultrasound, stirring, mode of oscillation Change molybdenum powder body to be sufficiently mixed in water and/or organic solvent;And/or the oligomer of phenylamine and/or oligomer of phenylamine derivative bag Include any one or any one the derivative in aniline tripolymer, Tetraaniline, aniline pentamer and the aggressiveness of aniline six; Preferably, the oligomer of phenylamine derivative includes the micromolecular compound containing oligomer of phenylamine, and particularly preferred self-contained aniline is oligomeric Thing is grafted or the polymer of block, particularly preferably the oligomer of phenylamine derivative from carboxy blocking or alkyl-substituted oligomer of phenylamine Derivative, particularly preferably from the compound with following any chemical formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic;And/or the two-dimentional molybdenum disulfide nano material be thickness be 1~ 20nm molybdenum disulfide two-dimensional nano piece.
  10. 10. a kind of molybdenum disulfide dispersion, it is characterised in that include:Decentralized medium;And it is scattered in the decentralized medium , compound as any one of claim 3-4.
  11. 11. molybdenum disulfide dispersion according to claim 10, it is characterised in that:The molybdenum disulfide dispersion is fluid Shape dispersion, preferably liquid dispersion or slurry;And/or the decentralized medium includes water, organic solvent and macromolecule resin In any one or two or more combinations;And/or the molybdenum disulfide dispersion includes below 10mg/mL curing Molybdenum, preferably comprise 0.1mg/mL~10mg/mL molybdenum disulfide, particularly preferably two comprising 0.1mg/mL~2.5mg/mL Molybdenum sulfide.
  12. A kind of 12. preparation method of molybdenum disulfide dispersion, it is characterised in that including:By molybdenum disulfide and oligomer of phenylamine and/or Oligomer of phenylamine derivative is uniformly mixed to form stabilising dispersions in decentralized medium;
    Preferably, oligomer of phenylamine and/or the oligomer of phenylamine derivative includes aniline tripolymer, Tetraaniline, aniline five Any one or any one derivative in aggressiveness and the aggressiveness of aniline six;Preferably, the oligomer of phenylamine derivative includes The polymer of micromolecular compound containing oligomer of phenylamine, particularly preferably self-contained oligomer of phenylamine grafting or block, particularly preferably certainly The oligomer of phenylamine derivative of carboxy blocking or alkyl-substituted oligomer of phenylamine derivative, particularly preferably there is following anyization certainly The compound of formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic;
    And/or the oligomer of phenylamine and/or the weight ratio preferably 0.1~10 of oligomer of phenylamine derivative and molybdenum disulfide:1, especially It is preferably 0.2~2:1;
    And/or the molybdenum disulfide is preferably two-dimentional molybdenum disulfide nano material, especially preferably thickness is the two of 1~20nm Molybdenum sulfide two-dimensional nano piece;
    And/or the decentralized medium includes water and/or organic solvent;
    And/or, it is preferred that the stabilising dispersions include below 10mg/mL molybdenum disulfide, particularly preferably comprising 0.1 Mg/mL~10mg/mL molybdenum disulfide, the further preferably molybdenum disulfide comprising 0.1mg/mL~2.5mg/mL.
  13. 13. a kind of redispersible molybdenum disulfide powder, it is characterised in that it is by removing any one of claim 10-11 Molybdenum disulfide dispersion in decentralized medium and the powder that obtains, and the powder can be directly scattered in again it is described scattered In medium.
  14. 14. a kind of molybdenum disulfide realized based on physical method disperses and redisperse method, it is characterised in that including:
    Molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative are uniformly mixed to form stable dispersion in decentralized medium Body,
    Remove the decentralized medium in the dispersion and obtain molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative Compound,
    And be scattered in the compound in decentralized medium again, stabilising dispersions are formed again;
    Preferably, oligomer of phenylamine and/or the oligomer of phenylamine derivative includes aniline tripolymer, Tetraaniline, aniline five Any one or any one derivative in aggressiveness and the aggressiveness of aniline six;Preferably, the oligomer of phenylamine derivative includes The polymer of micromolecular compound containing oligomer of phenylamine, particularly preferably self-contained oligomer of phenylamine grafting or block, particularly preferably certainly The oligomer of phenylamine derivative of carboxy blocking or alkyl-substituted oligomer of phenylamine derivative, particularly preferably there is following anyization certainly The compound of formula:
    Wherein, M includes H+、Na+、K+Or quaternary ammonium salt cationic;
    And/or, it is preferred that the decentralized medium includes water and/or organic solvent;
    And/or the molybdenum disulfide is preferably two-dimentional molybdenum disulfide nano material, especially preferably thickness is 1~20nm two sulphur Change molybdenum two-dimensional nano piece;
    And/or oligomer of phenylamine and/or the weight of oligomer of phenylamine derivative and molybdenum disulfide ratio are in the compound 0.1~10:1, preferably 0.2~2:1.
  15. 15. molybdenum disulfide is scattered and redisperse method, its feature exist for realizing based on physical method according to claim 14 In including:Molybdenum disulfide and oligomer of phenylamine and/or oligomer of phenylamine derivative are uniformly mixed to form surely in water/or organic solvent Determine dispersion liquid, the stable dispersions are dried with processing afterwards and forms the compound in powder shaped;At the drying The mode of reason is selected from least one of spray drying, rotary evaporation and vacuum drying.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671963A (en) * 2018-03-16 2018-10-19 浙江大学宁波理工学院 The preparation method of micro-/micro-nano structure cadmium sulfide/oligomer of phenylamine composite material
CN109943310A (en) * 2019-04-02 2019-06-28 侯吉瑞 A kind of modified MoS2Nano material and preparation method thereof
CN111019745A (en) * 2019-12-01 2020-04-17 苏州福瑞斯德新材料科技有限公司 MoS-containing2Water insoluble trace amount of lubricating fluid
CN111378520A (en) * 2019-12-01 2020-07-07 苏州福瑞斯德新材料科技有限公司 MoS-containing2Water soluble trace amount lubricating liquid
CN112359019A (en) * 2020-11-16 2021-02-12 苏州米苏生物技术有限公司 Chimeric antigen receptor T cell culture medium composition for resisting drug inhibition and application thereof
CN114171475A (en) * 2021-11-29 2022-03-11 微龛(广州)半导体有限公司 SOI wafer with heat dissipation structure and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254429A (en) * 2013-05-21 2013-08-21 合肥工业大学 Preparation method of polyaniline and molybdenum disulfide intercalated composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254429A (en) * 2013-05-21 2013-08-21 合肥工业大学 Preparation method of polyaniline and molybdenum disulfide intercalated composite material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MERCOURI G. KANATZIDIS ET AL.: "New Intercalation Compounds of Conjugated Polymers. Encapsulation of Polyaniline in MoS2", 《CHEM. MATER.》 *
RABIN BISSESSUR ET AL.: "Novel alkyl substituted polyanilines/molybdenum disulfide nanocomposites", 《MATERIALS CHEMISTRY AND PHYSICS》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671963A (en) * 2018-03-16 2018-10-19 浙江大学宁波理工学院 The preparation method of micro-/micro-nano structure cadmium sulfide/oligomer of phenylamine composite material
CN108671963B (en) * 2018-03-16 2021-10-22 浙江大学宁波理工学院 Preparation method of micro/nano structured cadmium sulfide/aniline oligomer composite material
CN109943310A (en) * 2019-04-02 2019-06-28 侯吉瑞 A kind of modified MoS2Nano material and preparation method thereof
CN109943310B (en) * 2019-04-02 2022-05-24 侯吉瑞 Modified MoS2Nano material and preparation method thereof
CN111019745A (en) * 2019-12-01 2020-04-17 苏州福瑞斯德新材料科技有限公司 MoS-containing2Water insoluble trace amount of lubricating fluid
CN111378520A (en) * 2019-12-01 2020-07-07 苏州福瑞斯德新材料科技有限公司 MoS-containing2Water soluble trace amount lubricating liquid
CN112359019A (en) * 2020-11-16 2021-02-12 苏州米苏生物技术有限公司 Chimeric antigen receptor T cell culture medium composition for resisting drug inhibition and application thereof
CN114171475A (en) * 2021-11-29 2022-03-11 微龛(广州)半导体有限公司 SOI wafer with heat dissipation structure and preparation method thereof

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