CN107464652A - A kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof - Google Patents

A kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof Download PDF

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CN107464652A
CN107464652A CN201710744329.2A CN201710744329A CN107464652A CN 107464652 A CN107464652 A CN 107464652A CN 201710744329 A CN201710744329 A CN 201710744329A CN 107464652 A CN107464652 A CN 107464652A
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mfe
flow liquid
magnetic flow
magnetic
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王光硕
马莹莹
崔国华
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CHINA YONGNIAN STANDARD COMPONENT RESEARCH INSTITUTE
Hebei University of Engineering
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CHINA YONGNIAN STANDARD COMPONENT RESEARCH INSTITUTE
Hebei University of Engineering
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/447Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids characterised by magnetoviscosity, e.g. magnetorheological, magnetothixotropic, magnetodilatant liquids
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

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Abstract

The present invention relates to novel intelligent field of magnetic material, specially a kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof.The present invention prepares amino modified individual layer molybdenum disulfide (MoS using lithium chloride chemical stripping method first2) nanometer sheet, carboxy-modified MFe is prepared using microwave chemical method2O4(M=Fe, Co and Ni) magnetic nano-particle, the reaction of amido link is then formed using amino and carboxyl by MFe2O4Nano-particle is uniformly assembled in MoS2Nanometer sheet surface (MoS2/MFe2O4), centrifuge and remove bottom sediment thing, the MoS for taking upper solution to be stablized2/MFe2O4Composite aqueous magnetic flow liquid.This method has the advantages of operating process is controllable, process repeatability is strong and is easy to large-scale production, and gained aqueous phase magnetic flow liquid has the advantages that null field viscosity is low, shear stress is big, sedimentation stability is good and use temperature range is wide.

Description

A kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof
Technical field
The present invention relates to novel intelligent field of magnetic material, specially a kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and Its preparation method.
Background technology
Rabinow in 1948 first proposed relevant magnetic flow liquid (Magnetorheological fluids, MRF) Concept, as typical intellectual material, it is a model of soft magnetic materials application.Magnetic flow liquid is to disperse soft magnetic particles The suspension liquid formed into carrier fluid, it is because magnetic flow liquid can exist quickly and reversibly why to be referred to as intellectual material Realize liquid to being similar to change between solid-state under external magnetic field control.In the case of null field, magnetic flow liquid shows as mobile performance Good liquid, its apparent viscosity very little;It can increase by two in short time (Millisecond) interior apparent viscosity under strong magnetic field action More than the order of magnitude, and class solid property is presented;And this change is continuous, reversible, that is, returned to again after removing magnetic field State originally.But from the fifties to the eighties during, due to the shear stress of not recognizing it potentiality and deposit Suspension, the corrosivity the problems such as, magnetic flow liquid development is very slow always.Into the nineties, with the raising of technology of preparing, Life has been shone in magnetic flow liquid research again, turns into an important branch of current intellectual material research field, and in engineering The application in field is magnetorheological by more and more extensive concern and research, including magnetorheological damping device, magnetorheological control device Polishing and magnetorheological sealing etc..
Most currently used for magnetic flow liquid base fluid is silicone oil, water and various mineral oil of different viscosities etc..Using oil as base The magnetic flow liquid of liquid can effectively slow down the sedimentation of magnetic-particle because base fluid viscosity itself is relatively large;Other oil is not Volatile, chemical stability is higher, is advantageous to improve the stability of magnetic flow liquid;But its shortcoming is oil during long-term use Class material can polymerize, aging, bacterial reproduction and inflammable.And though the magnetic flow liquid using water as base fluid can overcome lacking for oils base fluid Point, but its own viscosity is extremely low, and magnetic particle sedimentation is fast;The water capacity is easily evaporated, and is unfavorable for long-term use, and stability is poor.Water base magnetic The advantage of rheology liquid is that cost is low, nontoxic pollution-free, it is recyclable and MRF etc. have can not replace The advantage in generation.
Although traditional oxo iron powder magnetic flow liquid with prominent mechanical property to meet application requirement, but magnetic particle Settlement issues caused by density contrast between carrier fluid fail to be well solved always, extensive which has limited magnetic flow liquid Using.From the point of view of the method for existing improvement magnetorheological fluid sedimentation stability, using the addition additive such as nano-particle or anti-settling agent The system of magnetic flow liquid is complicated, and increases its null field viscosity, it is unfavorable to practical application;Using special base fluid such as density The larger ionic liquid of larger magnetic fluid or viscosity equally produces the problem of magnetic flow liquid null field viscosity increase, while cost is big It is big to improve.Therefore, the study hotspot of present magnetic flow liquid can be turned into by how taking into account magnetorheological fluid sedimentation stability and rheomagnetic And difficult point.
The content of the invention
It is an object of the invention to provide a kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof, by using The less layer structure composite magnetic particle of density, can effectively reduce the density contrast between dispersed phase and carrier fluid, not damage While magnetorheological fluid performance improve suspension sedimentation stability, gained aqueous phase magnetic flow liquid have null field viscosity it is low, shearing It should uprise, the advantages that sedimentation stability is good and use temperature range is wide.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows:
A kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid, using water as carrier fluid, with by amination individual layer MoS2Nanometer sheet and Carboxylated MFe2O4The MoS of the compound composition of magnetic nano-particle2/MFe2O4Magnetic coupling particle is that dispersed phase is dispersed in carrier fluid In, M is divalent metal.
One kind as the present invention is preferred, the MFe2O4Magnetic nano-particle is uniformly modified in individual layer MoS2Nanometer sheet table Face.
Another kind as the present invention is preferred, the MFe2O4In M=Fe or Co or Ni.
Another as the present invention is preferred, the MoS2/MFe2O4Magnetic coupling particle accounts for the quality of water based magnetic rheologic liquid Fraction is 5-45wt%.
Another as the present invention is preferred, the carboxylated MFe2O4A diameter of 3-25nm of magnetic nano-particle, its shape Shape is spherical or spherical;The thickness of the amination individual layer MoS2 nanometer sheets is 0.5-20nm, and it is shaped as individual layer and peels off knot Structure, size are 0.5-10 μm, its shared described MoS2/MFe2O4Magnetic coupling granular mass percentage composition is 0.5-60wt%.
Above-mentioned technical proposal passes through carboxylated MFe2O4Magnetic nano-particle is equably modified in individual layer two by acid amides bonding Around molybdenum oxide nanometer sheet, MoS is formed2/MFe2O4Magnetic coupling particle, using MoS2/MFe2O4Magnetic coupling particle replaces passing The magnetic-particle of system prepares magnetic flow liquid, uses MoS2For typical multi-layer sheet structure, there is good mechanical property, and can make For the antiprecipitant, antiwear additive and lubricant of magnetic flow liquid;And MoS2/MFe2O4Magnetic coupling grain density is smaller, as Dispersed phase, the density contrast between dispersed phase and carrier fluid can be effectively reduced, be improved while magnetorheological fluid performance is not damaged outstanding The sedimentation stability and structural stability of supernatant liquid;By MFe2O4Magnetic nano-particle controllable load is in individual layer MoS2Nanometer sheet surface, This is allowed under additional magnetic fields, MoS2/MFe2O4Magnetic coupling particle arranges along magnetic direction ordering rule, can be significantly The shear stress of water based magnetic rheologic liquid made from raising and other rheomagnetic energy.
Present invention also offers prepare this MoS2/MFe2O4The preparation method of composite aqueous magnetic flow liquid, including following step Suddenly,
(1) amination individual layer molybdenum disulfide (MoS2) nanometer sheet preparation,
By MoS2Powder is added in the deionized water of certain volume, is subsequently added into a certain amount of lithium salts, sonic oscillation, then Amino modified dose is added, mechanical agitation, by its reaction product by washing, being collected by centrifugation, dry, obtains amination individual layer MoS2 Nanometer sheet;
(2) carboxylated MFe2O4The preparation of magnetic nano-particle,
The trivalent iron salt of proportional metering and divalence M salt are dissolved in the deionized water of certain volume, nitrogen bubble is gone Except the dissolved oxygen in solution, after mechanical agitation is uniform, it is 10-14 that highly basic regulation system pH value, which is added dropwise, is placed in microwave reactor, instead Carboxy-modified dose is added after should terminating, is reacted under mechanical agitation, reaction receives its reaction product by washing, centrifugation after terminating Collection, dry, obtain carboxylated MFe2O4Magnetic nano-particle;
(3)MoS2/MFe2O4The preparation of composite aqueous magnetic flow liquid,
By amination individual layer MoS obtained above2Nanometer sheet and carboxylated MFe2O4Nano-particle is scattered in by a certain percentage In the deionized water of certain volume, catalyst is added, reacts and MoS is made2/MFe2O4Magnetic coupling particle, centrifuge and remove bottom Layer sediment, takes upper solution to produce stable individual layer MoS2/MFe2O4Composite aqueous magnetic flow liquid.
Such scheme step adds lithium salts in (1) in the solution dissolved with molybdenum dioxide, is in order to which lithium ion is inserted into In the molybdenum dioxide of stratiform so that molybdenum dioxide is easier to be modified by ferrite, and lithium salts is preferably lithium chloride;Add the molten of lithium salts Liquid improves lithium ion intercalation yield by sonic oscillation, and amino modified dose is successfully incorporated into amino in molybdenum dioxide.
Highly basic in step (2) is preferably sodium hydroxide solution, and the solution after PH is regulated is placed into microwave reactor In, accelerate reaction speed so that the seed activity being prepared is higher, improves reaction yield.
Catalyst in step (3) is preferably N, N'- Dicyclohexylcarbodiimides, with MoS2The mass ratio of nanometer sheet is 20:1.
Preferably, the reaction condition in step (1) is sonic oscillation 1-5h to one kind as the present invention, mechanical agitation 1-4h, Its reaction product is washed three times with deionized water and absolute ethyl alcohol, and 24h is dried in vacuum drying chamber;Reaction bar in step (2) Part is nitrogen bubble 0.5h, mechanical agitation 0.5h, to be placed in microwave reactor and react 10min, mechanical agitation 1-4h, and it reacts Product is rinsed three times respectively with deionized water and ethanol, is placed in vacuum drying chamber and is dried 24h.
Preferably, amino modified dose used in the step (1) is octadecylamine second to another kind as the present invention One kind in hydrochlorate, coconut amine acetate, oleyl amine hydrochloride and hydrogenated tallow amine hydrochlorate, wherein molybdenum disulfide nano sheet and ammonia The mass ratio of base modifying agent is 1-20:1.
Another as the present invention is preferred, and the trivalent iron salt used in the step (2) is hydrated for the chloride of iron One kind in thing, nitrate hydrate, sulfate hydrate, oxalic acid salt hydrate, acetic acid salt hydrate, used divalence M Salt is one in M chloride hydrates, nitrate hydrate, sulfate hydrate, oxalic acid salt hydrate, acetic acid salt hydrate Kind, wherein the mol ratio of trivalent iron salt and divalence M salt is 2:1.
Another as the present invention is preferred, and the microwave reactor power used in the step (2) is 600W.
Another as the present invention is preferred, and carboxy-modified dose used in the step (2) is sodium alginate, pectin One kind in sour sodium, sodium humate and cluck ton natural gum, wherein trivalent iron salt and carboxy-modified dose of mass ratio are 1-20:1.
The method applied in the present invention has the advantages of preparation time is short, operating process is simple and is easy to large-scale production, Gained water based magnetic rheologic liquid has the advantages that null field viscosity is low, shear stress is big, sedimentation stability is good and use temperature range is wide.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description;
Fig. 1 is MoS in embodiment 12/Fe3O4The X-ray diffracting spectrum of magnetic coupling particle;
Fig. 2 is MoS in embodiment 12/Fe3O4The room temperature magnetization curve of magnetic coupling particle;
Fig. 3 is MoS in embodiment 12/Fe3O4Composite aqueous magnetic flow liquid viscosity is under different magnetic field with the change of shear rate Change graph of a relation;
Fig. 4 is MoS in embodiment 12/Fe3O4Composite aqueous magnetic flow liquid shear stress is under different magnetic field with shear rate Variation relation figure;
Fig. 5 is MoS in embodiment 12/Fe3O4The settlement stability linearity curve of composite aqueous magnetic flow liquid.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Ground describes, it is clear that described embodiment is only the part of the embodiment of the present invention, rather than whole embodiments.Based on this Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made Example is applied, belongs to the scope of protection of the invention.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still the present invention can be with It is different from other manner described here using other to implement, those skilled in the art can be without prejudice to intension of the present invention In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Embodiment 1
(1) amination individual layer molybdenum disulfide (MoS2) nanometer sheet preparation
450mL deionized waters, 1.0g commercializations MoS will be added in 1000mL three-necked flask2Powder and 0.5g lithium chlorides, put In low power ultrasound groove, sonic oscillation 1h, 0.25g octadecyl amine acetates are then added, mechanical agitation 1h, it reacts production Thing is washed with deionized three times, is collected by centrifugation, and is subsequently placed in vacuum drying chamber and dries 24h, obtains amination individual layer MoS2 Nanometer sheet.
(2) carboxylated Fe3O4The preparation of magnetic nano-particle
By 12g FeCl in 1000mL three-necked flask3·6H2O and 4.43g FeCl2·4H2O is dissolved in 750mL and gone Ionized water, the dissolved oxygen in solution is removed with nitrogen bubble 0.5h, 100mL 3.5M sodium hydroxide solution, which is gradually added dropwise, to be made instead It is 12 to answer system pH, is placed in 600W microwave reactors and reacts 10min, then adds 1.8g sodium alginate, mechanical agitation Being centrifuged after 4h, its reaction product is rinsed three times respectively with deionized water and ethanol, is placed in vacuum drying chamber and is dried 24h, Obtain carboxylated Fe3O4Magnetic nano-particle.
(3)MoS2/Fe3O4The preparation of composite aqueous magnetic flow liquid
By amination MoS obtained by above-mentioned steps2Nanometer sheet and carboxylated Fe3O4Nano-particle is scattered in going for certain volume In ionized water, mechanical agitation 12h after 1.75g N, N'- Dicyclohexylcarbodiimides is added, centrifuges and removes bottom sediment thing, Upper solution is taken to produce stable individual layer MoS2/Fe3O4Composite aqueous magnetic flow liquid.Wherein, MoS2Nanometer sheet is in MoS2/Fe3O4 Shared mass fraction is 13.1%, MoS in composite particles2/Fe3O4Composite particles account for the 5wt% of water based magnetic rheologic liquid.
Embodiment 2
(1) amination individual layer molybdenum disulfide (MoS2) nanometer sheet preparation
750mL deionized waters, 3.0g commercializations MoS will be added in 1000mL three-necked flask2Powder and 1.5g lithium chlorides, put In low power ultrasound groove, sonic oscillation 2h, 0.75g octadecyl amine acetates, mechanical agitation 1h, gained reaction are then added Product is washed with deionized three times, is collected by centrifugation, and is subsequently placed in vacuum drying chamber and dries 24h, obtains amination individual layer MoS2Nanometer sheet.
(2) carboxylated CoFe2O4The preparation of magnetic nano-particle
By 16.0g FeCl in 1000mL three-necked flask3·6H2O and 8.1g CoCl2·6H2O is dissolved in 750mL and gone Ionized water, the dissolved oxygen in solution is removed with nitrogen bubble 0.5h, 120mL 3.5M sodium hydroxide solution, which is gradually added dropwise, to be made instead It is 12 to answer system pH, is placed in 600W microwave reactors and reacts 10min, then adds 2.3g sodium alginate, mechanical agitation Being centrifuged after 4h, its reaction product is rinsed three times respectively with deionized water and ethanol, is placed in vacuum drying chamber and is dried 24h, Obtain carboxylated CoFe2O4Magnetic nano-particle.
(3)MoS2/CoFe2O4The preparation of composite aqueous magnetic flow liquid
By amination MoS obtained by above-mentioned steps2Nanometer sheet and carboxylated CoFe2O4Nano-particle is scattered in certain volume In deionized water, mechanical agitation 12h after 1.75g N, N'- Dicyclohexylcarbodiimides is added, centrifuges and removes bottom sediment Thing, upper solution is taken to produce stable individual layer MoS2/CoFe2O4Composite aqueous magnetic flow liquid.Wherein, MoS2Nanometer sheet is in MoS2/ CoFe2O4Shared mass fraction is 27.4%, MoS in composite particles2/CoFe2O4Composite particles account for water based magnetic rheologic liquid 20wt%.
Embodiment 3
(1) amination individual layer molybdenum disulfide (MoS2) nanometer sheet preparation
1000mL deionized waters, 6.0g commercializations MoS will be added in 1000mL three-necked flask2Powder and 3.0g lithium chlorides, It is placed in low power ultrasound groove, sonic oscillation 4h, then addition 1.5g octadecyl amine acetates, mechanical agitation 1h, gained are anti- Answer product to be washed with deionized three times, be collected by centrifugation, be subsequently placed in vacuum drying chamber and dry 24h, obtain amination individual layer MoS2Nanometer sheet.
(2) carboxylated NiFe2O4The preparation of magnetic nano-particle
By 20.0g FeCl in 1000mL three-necked flask3·6H2O and 8.81g NiCl2·6H2O is dissolved in 750mL Deionized water, the dissolved oxygen in solution is removed with nitrogen bubble 0.5h, 150mL 3.5M sodium hydroxide solution, which is gradually added dropwise, to be made PH value of reaction system is 12, is placed in 600W microwave reactors and reacts 10min, then adds 3.2g sodium alginate, and machinery stirs Centrifuged after mixing 4h, its reaction product is rinsed three times respectively with deionized water and ethanol, is placed in vacuum drying chamber and is dried 24h, obtain carboxylated NiFe2O4Magnetic nano-particle.
(3)MoS2/NiFe2O4The preparation of composite aqueous magnetic flow liquid
By amination MoS obtained by above-mentioned steps2Nanometer sheet and carboxylated NiFe2O4Nano-particle is scattered in certain volume In deionized water, mechanical agitation 12h after 1.75g N, N'- Dicyclohexylcarbodiimides is added, centrifuges and removes bottom sediment Thing, upper solution is taken to produce stable MoS2/NiFe2O4Composite aqueous magnetic flow liquid.Wherein, MoS2Nanometer sheet is in MoS2/ NiFe2O4Shared mass fraction is 40.8%, MoS in composite particles2/NiFe2O4Composite particles account for water based magnetic rheologic liquid 45wt%.
Obtained MoS in above-mentioned implementation 12/Fe3O4The performance characterization of composite aqueous magnetic flow liquid is as follows:
Fig. 1 is the X-ray diffracting spectrum of MoS2/Fe3O4 magnetic coupling particles in embodiment 1.It can be observed from figure, Occur strong characteristic diffraction peak at 2 θ=30.1 °, 35.4 °, 42.7 °, 53.3 °, 56.9 ° and 62.4 °, correspond to four oxygen respectively Change (220), (311), (400), (422), (511) and (440) crystal face in three-iron normal data (JCPDS No.22-1086). In addition, in MoS2/Fe3O4 composite particles in addition to the characteristic peak of ferroso-ferric oxide, also can substantially be observed at 2 θ=14.8 ° To the characteristic peak of molybdenum disulfide nano sheet, result above shows the successful preparation of MoS2/Fe3O4 composite particles.
Fig. 2 is the room temperature magnetization curve of MoS2/Fe3O4 magnetic coupling particles in embodiment 1.It can be seen that MoS2/ Typical S types curve is presented in the magnetization curve of Fe3O4 composite particles, meets Langevin equation.In addition, compound of MoS2/Fe3O4 Do not occur obvious hysteresis curve on the magnetization curve of grain, remanent magnetism and coercivity are substantially zeroed, show compound of MoS2/Fe3O4 Grain has superparamagnetism, saturation magnetization 60.3emu/g at room temperature.
Fig. 3 be embodiment 1 in the composite aqueous magnetic flow liquid viscosity of MoS2/Fe3O4 under different magnetic field with shear rate Variation relation figure.Under null field state, the magnetic flow liquid of preparation, which has higher initial viscosity and shows slight shearing, to be become Dilute phenomenon, as the increased viscosity of shear rate reduces rapidly and gradually tends towards stability.After applying external magnetic field, the magnetic current of preparation The viscosity for becoming liquid significantly increases in whole range of shear rate, and the bigger viscosity of magnetic field intensity is bigger, and shows brighter Aobvious shear shinning phenomenon.
Fig. 4 is that the composite aqueous magnetic flow liquid shear stresses of MoS2/Fe3O4 are fast with shearing under different magnetic field in embodiment 1 The variation relation figure of rate.As seen from the figure, the shear stress of the magnetic flow liquid of preparation increases with the increase of shear rate.Identical Under shear rate, its shear stress increases with the increase of magnetic field intensity, shows significant magnetic rheology effect.
Fig. 5 is the settlement stability linearity curve of the composite aqueous magnetic flow liquids of MoS2/Fe3O4 in embodiment 1.With traditional carbonyl Iron powder (CI) magnetic flow liquid is compared, the sedimentation speed of the composite aqueous magnetic flow liquids of MoS2/Fe3O4 of preparation within 15 day sedimentation time Rate is slower, shows more excellent sedimentation stability.On the one hand, individual layer MoS2 nanometer sheets have unique layer structure, can be with The effect similar to parachute is played so as to improve the sedimentation stability of magnetic flow liquid.On the other hand, MoS2/Fe3O4 composite particles With less density, the density contrast between dispersed phase and carrier fluid can be reduced, so as to effectively improve the heavy of gained magnetic flow liquid Stability drops.

Claims (10)

  1. A kind of 1. MoS2/MFe2O4Composite aqueous magnetic flow liquid, it is characterised in that:Using water as carrier fluid, with by amination individual layer MoS2 Nanometer sheet and carboxylated MFe2O4The MoS of the compound composition of magnetic nano-particle2/MFe2O4Magnetic coupling particle is that dispersed phase uniformly divides It is dispersed in carrier fluid, M is divalent metal.
  2. A kind of 2. MoS according to claim 12/MFe2O4Composite aqueous magnetic flow liquid, it is characterised in that:The MFe2O4 Magnetic nano-particle is uniformly modified in individual layer MoS2Nanometer sheet surface.
  3. A kind of 3. MoS according to claim 1 or 22/MFe2O4Composite aqueous magnetic flow liquid, it is characterised in that:It is described MFe2O4In M=Fe or Co or Ni.
  4. A kind of 4. MoS according to claim 32/MFe2O4Composite aqueous magnetic flow liquid, it is characterised in that:The MoS2/ MFe2O4The mass fraction that magnetic coupling particle accounts for water based magnetic rheologic liquid is 5-45wt%.
  5. 5. according to a kind of MoS described in claim 1 or 2 or 32/MFe2O4Composite aqueous magnetic flow liquid, it is characterised in that:It is described Carboxylated MFe2O4A diameter of 3-25nm of magnetic nano-particle, it is shaped as spherical or spherical;The amination individual layer MoS2 The thickness of nanometer sheet is 0.5-20nm, and it is shaped as individual layer lift-off structure, and size is 0.5-10 μm, its shared described MoS2/ MFe2O4Magnetic coupling granular mass percentage composition is 0.5-60wt%.
  6. A kind of 6. MoS2/MFe2O4Its preparation method of composite aqueous magnetic flow liquid, it is characterised in that:Comprise the following steps,
    (1) amination individual layer molybdenum disulfide (MoS2) nanometer sheet preparation,
    By MoS2Powder is added in the deionized water of certain volume, is subsequently added into a certain amount of lithium salts, sonic oscillation, is then added Amino modified dose, mechanical agitation, by its reaction product by washing, being collected by centrifugation, dry, obtain amination individual layer MoS2Nanometer Piece;
    (2) carboxylated MFe2O4The preparation of magnetic nano-particle,
    The trivalent iron salt of proportional metering and divalence M salt are dissolved in the deionized water of certain volume, nitrogen bubble, machinery stirs After mixing uniformly, it is 10-14 that highly basic regulation system pH value, which is added dropwise, is placed in microwave reactor, and reaction adds carboxy-modified dose after terminating, Reacted under mechanical agitation, reaction, which passes through its reaction product after terminating, washs, is collected by centrifugation, drying, and obtains carboxylated MFe2O4Magnetic Property nano-particle;
    (3)MoS2/MFe2O4The preparation of composite aqueous magnetic flow liquid,
    By amination individual layer MoS obtained above2Nanometer sheet and carboxylated MFe2O4Nano-particle is scattered in necessarily by a certain percentage In the deionized water of volume, catalyst is added, reacts and MoS is made2/MFe2O4Magnetic coupling particle, centrifuge removal bottom and sink Starch, upper solution is taken to produce stable individual layer MoS2/MFe2O4Composite aqueous magnetic flow liquid.
  7. A kind of 7. MoS according to claim 62/MFe2O4The preparation method of composite aqueous magnetic flow liquid, it is characterised in that: Reaction condition in step (1) is sonic oscillation 1-5h, mechanical agitation 1-4h, its reaction product deionized water and anhydrous second Alcohol is washed three times, and 24h is dried in vacuum drying chamber;Reaction condition in step (2) is nitrogen bubble 0.5h, mechanical agitation 0.5h, it is placed in microwave reactor and reacts 10min, mechanical agitation 1-4h, its reaction product is rushed respectively with deionized water and ethanol Wash three times, be placed in vacuum drying chamber and dry 24h.
  8. A kind of 8. MoS according to claim 6 or 72/MFe2O4The preparation method of composite aqueous magnetic flow liquid, its feature exist In:Amino modified dose used in the step (1) is octadecyl amine acetate, coconut amine acetate, oleyl amine hydrochloride With one kind in hydrogenated tallow amine hydrochlorate, wherein molybdenum disulfide nano sheet and amino modified dose of mass ratio is 1-20:1.
  9. A kind of 9. MoS according to claim 62/MFe2O4The preparation method of composite aqueous magnetic flow liquid, it is characterised in that: Trivalent iron salt used in the step (2) is chloride hydrates, nitrate hydrate, sulfate hydrate, the grass of iron One kind in hydrochloride hydrates, acetic acid salt hydrate, used divalence M salt are M chloride hydrates, nitrate hydration One kind in thing, sulfate hydrate, oxalic acid salt hydrate, acetic acid salt hydrate, wherein mole of trivalent iron salt and divalence M salt Than for 2:1.
  10. A kind of 10. MoS according to claim 62/MFe2O4The preparation method of composite aqueous magnetic flow liquid, its feature exist In:Microwave reactor power used in the step (2) is 600W.
CN201710744329.2A 2017-08-25 2017-08-25 A kind of MoS2/MFe2O4Composite aqueous magnetic flow liquid and preparation method thereof Pending CN107464652A (en)

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Cited By (1)

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CN115634699A (en) * 2022-11-07 2023-01-24 浙江省环境科技有限公司 Nickel-doped CoFe composite oxide/molybdenum disulfide supported catalyst and preparation and application thereof

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Application publication date: 20171212