CN106634134A - Preparation of magnetic ferroferric oxide/graphene composite material and application thereof in preparing magnetic paint - Google Patents
Preparation of magnetic ferroferric oxide/graphene composite material and application thereof in preparing magnetic paint Download PDFInfo
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- CN106634134A CN106634134A CN201610841583.XA CN201610841583A CN106634134A CN 106634134 A CN106634134 A CN 106634134A CN 201610841583 A CN201610841583 A CN 201610841583A CN 106634134 A CN106634134 A CN 106634134A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/23—Magnetisable or magnetic paints or lacquers
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Abstract
The invention discloses a preparation method of a magnetic ferroferric oxide/graphene composite material. The method comprises the following steps: ultrasonically dispersing graphite oxide into water to form graphite oxide dispersion liquid, adding ferroferric oxide into the graphite oxide dispersion liquid, and ultrasonically dispersing and uniformly mixing; dropwise adding ammonia water into a mixed system, so that pH of the mixed system is equal to 12 to 13, then adding a hydrazine hydrate solution, and ultrasonically treating for 1 to 2 min; and transferring the system into a reaction kettle, reacting for 10 to 12 h at 160 to 180 DEG C, cooling to the room temperature, washing, and drying to obtain the ferroferric oxide/graphene composite material. By virtue of test, the composite material has good dispersity, so that the composite material can be used for preparing magnetic paint, and further preparing an electromagnetic shielding layer.
Description
Technical field
The present invention relates to a kind of preparation of magnetic ferroferric oxide/graphene composite material, more particularly to one kind is aoxidizing
Graphite and ferroso-ferric oxide are raw material, by the method for hydro-thermal method one-step synthesis magnetic ferroferric oxide/graphene composite material；
The present invention also relates to application of the composite of said method preparation in magnetic paint is prepared, and belongs to composite and film
Field of material technology.
Background technology
Graphene is sp2The flat film of the fine and close monolayer bi-dimensional cellular shape structure that the carbon atom of bonding is constituted.From 2004
Since year finds, because its outstanding physical property, thermal property, optical property and electric property receive extensive pass
Note.The thermoelectricity conductance of Graphene can reach 3000 ~ 5000Wm-1K-1, it is ten times of copper.At room temperature electron mobility is about
10 000cm2V-1s-1, exceeded CNT and monocrystal silicon.The thickness of Graphene is only 0.35nm, but specific surface area is up to
2600m2 g-1, thus be a kind of extremely excellent material.
Ferroso-ferric oxide belongs to cubic system, inverse spinel structure, with excellent Magnetics characteristL so as in magnetic storage material
The aspect such as material, microwave absorption, sapecial coating, drug targeting guiding, magnetic multifunctional composite, catalyst and biological engineering has weight
The application wanted.Especially in recent years the memory density of magnetic memory materials is improved rapidly, and the superparamagnetism of magnetic material and magnetic ring
Answering property receives the especially concern of people.Meanwhile, magnetic ferroferric oxide nano-particles of the synthesis with biological safety are because of it
Become research in the wide application prospect of the biomedical sector such as cell separation, targeted drug, nuclear magnetic resonance and magnetic thermotherapy
One of focus.
Graphene can effectively reduce the agglomeration of ferroso-ferric oxide with ferriferrous oxide composite material, increase its ratio
Surface area and electric conductivity, thus it is of great interest.CN201210005172.9 discloses a kind of magnetic Nano four
The preparation method of Fe 3 O-graphene composite catalyst, be by graphite oxide ultrasonic disperse in ethanol and aqueous systems；Again will
Solubility trivalent iron salt and divalent iron salt are disperseing in ethanol, to be then added to the alcohol-water body of graphite oxide ultrasound respectively
In system, after 50 ~ 90 DEG C, add ammonia to adjust pH and reacted for 9 ~ 11；Product carries out Magneto separate, is washed with deionized, and does
Magnetic nanometer ferroferric oxide-graphene composite catalyst is obtained after dry.Nano ferriferrous oxide-Graphene prepared by the method
Composite catalyst granular size is homogeneous, be uniformly dispersed, magnetic is preferable.But, ferroso-ferric oxide-Graphene obtained in the method phase
Composite is tridimensional network due to Graphene therein, so being only applicable to the less paint of viscosity, is added into
Dispersion can be caused uneven in too sticky paint.
Magnetic is painted, and is, with varnish as base material, to add made by pigment grind, coating be dried after in magneto-optic color and film
Hard, conventional has phenolic enamel and the class of synthetic enamel two, is suitable for metal window yarn network etc..
The content of the invention
The purpose of the present invention is for problems of the prior art, there is provided prepare magnetic by a kind of step of hydro-thermal method one
The method of property ferroso-ferric oxide/graphene composite material；
It is a further object of the present invention to provide magnetic ferroferric oxide/graphene composite material prepared by said method is preparing magnetic
Property paint in application.
First, the preparation of magnetic ferroferric oxide/graphene composite material
The method that the present invention prepares magnetic ferroferric oxide/graphene composite material, be by graphite oxide ultrasonic disperse in water
Graphite oxide dispersion is formed, by ferroso-ferric oxide（Particle diameter is 20 ~ 30nm）In adding graphite oxide dispersion, ultrasound mixes it
Close uniform；Again to Deca ammonia in mixed system, pH=12 ~ 13 of mixed system are made, be subsequently adding hydrazine hydrate solution, ultrasound 1 ~
2min；System is transferred in reactor, in 160 ~ 180 DEG C 10 ~ 12h is reacted, be cooled to room temperature, washed, be dried, obtain four oxygen
Change three-iron/graphene composite material.
Ferroso-ferric oxide is 2 with the mass ratio of graphite oxide:1~4:1.The amount of ferroso-ferric oxide should not be excessive, otherwise can
Generation agglomeration.
In graphite oxide dispersion, the content of graphite oxide is 1 ~ 1.5mg/mL；The mass percent of hydrazine hydrate solution is
40~80%；Graphite oxide dispersion is 8 with the volume ratio of hydrazine hydrate solution:1~9:1.
The drying is vacuum dried at 60 ~ 70 DEG C.
2nd, the pattern and property of magnetic ferroferric oxide/graphene composite material
The ferroso-ferric oxide for below by X-ray diffraction analysis, scanning electron microscope analysis, transmission electron microscope analysis being prepared by the present invention/
The structure and pattern of graphene composite material is analyzed explanation.
1st, X-ray diffraction analysis
Fig. 1 is the X-ray diffractogram that the present invention prepares ferroso-ferric oxide/graphene composite material.The feature presented from figure is spread out
Penetrating peak and can be seen that prepared composite has complete crystalline state.Wherein 2 θ angles be 18.32 °, 30.12 °, 35.44 °,
The diffraction maximum occurred at 37.12 °, 43.12 °, 53.4 °, 57 ° and 62.5 ° show that peak position is identical right with ferroso-ferric oxide standard
111,220,200,311,222,400,422,511 and 440 crystal faces of ferroso-ferric oxide are answered, diffraction maximum is stone at 2 θ=24.5 °
002 crystal face characteristic diffraction peak of black alkene, shows that graphite oxide has been reduced for Graphene.
2nd, scanning electron microscope analysis
Fig. 2 is that the response time is sweeping for ferroso-ferric oxide obtained in 12h/30000 times of graphene composite material amplification at 180 DEG C
Retouch Electronic Speculum（SEM）Figure.Can draw from figure, graininess（Particle diameter is 20 ~ 30nm）Ferroso-ferric oxide be distributed in netted graphite
The surface of alkene, part ferroso-ferric oxide is coated by Graphene, and the addition for illustrating Graphene effectively slow down ferroso-ferric oxide
Agglomeration.
3rd, Magnetic Test
Fig. 3 is the hysteresis graph of ferroso-ferric oxide/graphene composite material prepared by the present invention.Can draw from figure, stone
After black alkene is compound with ferroso-ferric oxide, product still has stronger magnetic, therefore can be used as a kind of magnetic material.
4th, the dispersibility in varnish.
Different scores are taken respectively（Ferroso-ferric oxide is 2 with the mass ratio of Graphene:1、4:1）Magnetic ferroferric oxide/graphite
Alkene composite 10mg, in being dispersed in 10mL varnish, ultrasound makes it be uniformly dispersed.Then observe it and ask dispersibility therein
Energy.As a result find, after standing 8 days, magnetic ferroferric oxide/graphene composite material is not settled, and illustrates composite clear
There is good dispersibility in paint, therefore, can be used to prepare magnetic paint.
3rd, the preparation of magnetic paint
Ferroso-ferric oxide/graphene composite material is added in ethanol with 1 ~ 1.5mg/mL, 10 ~ 15min of ultrasonic disperse；Again plus
Enter varnish, fully shaking, solution is layered, and abandoning supernatant continuously adds varnish, until solution is not stratified, obtain magnetic paint.
Due to the presence of magnetic ferroferric oxide in obtained paint, with good magnetic, can be used to prepare electromagnetic shielding material.
The present invention has advantages below relative to prior art：
1st, the present invention has been obtained graphene net parcel with graphite oxide and ferroso-ferric oxide as raw material by one step hydro thermal method
Ferriferrous oxide composite material, compared to the method that other prepare Graphene and three dimensional structure metal oxide composite, into
This relatively low, technique is simpler, reaction condition is gentle, it is pollution-free, be easy to large-scale production；
2nd, the present invention adds in preparation process without any other reactant, stable reaction conditions, therefore repeatability is high；
3rd, the composite that the present invention is obtained has good dispersibility in paint, therefore can be used to prepare magnetic paint, enters one
Step prepares coating for EMI shielding.
Description of the drawings
Fig. 1 is the X-ray diffractogram of composite（XRD）.
The scanning electron microscope (SEM) photograph of composite obtained in Fig. 2（SEM）.
Fig. 3 show the hysteresis graph of composite.
Specific embodiment
Below by instantiation to the preparation of flake graphite alkene coated ferroferric oxide composite of the present invention, structure,
Pattern etc. is described further.
Embodiment one
（1）The preparation of graphite oxide
0.5g crystalline flake graphites are weighed, 4.5g potassium permanganate is added to mix homogeneously in there-necked flask.Measure the addition of 7.5mL strong phosphoric acid
Beaker, measures 60mL concentrated sulphuric acids and is poured slowly in strong phosphoric acid.There-necked flask is placed in ice-water bath, is stirred.It is slowly added to above-mentioned
Nitration mixture, after stirring reaction 1h at 30 ~ 40 DEG C, is warming up to 50 DEG C and continues to react 12h.Reaction is cooled to room temperature after terminating, will be anti-
Answer product to be poured slowly in the frozen water containing 10mL hydrogen peroxide, stand, after removing supernatant, sucking filtration, with 5% hydrochloric acid come fully
Washing filter cake, until without SO in filtrate4 2-, subsequent deionized water and ethanol alternately washing to neutrality, in 50 DEG C of vacuum drying
The graphite oxide that 24h is obtained.
（2）The preparation of ferroso-ferric oxide
Take the water of 4.054g six and iron chloride and 2.78g green vitriols (wherein ferric ion and ferrous ion
Mol ratio is 3:2) it is respectively placed in the beaker of 50mL, respectively adds mixing after ultrapure water dissolution to be made into 120mL solution, logical nitrogen is removed
Add after oxygen in 250mL three-neck flasks, water-bath at 30 DEG C, mechanical agitation（Stir speed (S.S.) is 300r/min）, hold in course of reaction
It is continuous to be passed through nitrogen.It is 60 DEG C to adjust bath temperature, and with dropper ammonia and Polyethylene Glycol are added dropwise over.Stop after 30 ~ 35min anti-
Should, sample liquid is proceeded in beaker, 5 ~ 10min of ultrasonic disperse, natural cooling hatching 1h.Magnetic Isolation, respectively with ultra-pure water and nothing
Water-ethanol is washed 3 times, the graininess ferroso-ferric oxide for obtaining.
（3）The preparation of magnetic ferroferric oxide/graphene composite material
Take 25mg graphite oxides to be dissolved in 25mL distilled water, 10 ~ 15min of ultrasonic disperse；50mg ferroso-ferric oxide is added and is aoxidized
In graphite dispersing solution, 10 ~ 15min of ultrasound so as to mix homogeneously；3 ~ 5mL of Deca ammonia in mixture, makes the pH value of solution extremely
12 ~ 13 or so, then 3 ~ 5mL of Deca hydrazine hydrates thereto, 1 ~ 2min of ultrasound；Transfer reaction is reacted into reactor at 180 DEG C
12h, is cooled to room temperature, washing, is vacuum dried at 60 DEG C, obtains magnetic ferroferric oxide/graphene composite material.
（4）The preparation of magnetic ferroferric oxide/Graphene Compound paint
Magnetic ferroferric oxide/graphene composite material 10mg is taken, in being added to 10mL ethanol, 10 ~ 15min of ultrasonic disperse, to
Wherein Deca varnish, fully shaking, solution layering, abandoning supernatant（Ethanol）, continue Deca varnish, until solution is not stratified,
Obtain ferroso-ferric oxide/Graphene composite magnetic paint.
Embodiment two
（1）The preparation of graphite oxide：With example 1；
（2）The preparation of ferroso-ferric oxide：With example 1；
（3）The preparation of magnetic ferroferric oxide/graphene composite material：Take 25mg graphite oxides to be dissolved in 25mL distilled water, surpass
Sound disperses 10 ~ 15min；0.1g ferroso-ferric oxide is added in graphite oxide solution, 10 ~ 15min of ultrasound so as to mix homogeneously；
3 ~ 5mL of Deca ammonia in mixture, the pH value for making solution is 12 ~ 13 or so, then 3 ~ 5mL of Deca hydrazine hydrates thereto, ultrasound 1
~2min；Transfer reaction reacts 12h into reactor in 180 DEG C, is cooled to room temperature, washs, and is vacuum dried at 60 DEG C, obtains most
End-product.
（4）The preparation of magnetic paint：With example 1.
Claims (8)
1. a kind of preparation method of magnetic ferroferric oxide/graphene composite material, be by graphite oxide ultrasonic disperse in water
Graphite oxide dispersion is formed, ferroso-ferric oxide is added in graphite oxide dispersion, ultrasound makes its mix homogeneously；Again to mixing
Deca ammonia in system, makes pH=12 ~ 13 of mixed system, is subsequently adding hydrazine hydrate solution, 1 ~ 2min of ultrasound；System is shifted
Into reactor, 10 ~ 12h is reacted in 160 ~ 180 DEG C, be cooled to room temperature, washed, be dried, obtain ferroso-ferric oxide/Graphene multiple
Condensation material.
2. the preparation method of magnetic ferroferric oxide/graphene composite material as claimed in claim 1, it is characterised in that：Four oxygen
The particle diameter for changing three-iron is 20 ~ 30nm.
3. the preparation method of magnetic ferroferric oxide/graphene composite material as claimed in claim 1 or 2, it is characterised in that：Four
Fe 3 O is 2 with the mass ratio of graphite oxide:1~4:1.
4. the preparation method of magnetic ferroferric oxide/graphene composite material as claimed in claim 1 or 2, it is characterised in that：Oxygen
In graphite dispersion liquid, the content of graphite oxide is 1 ~ 1.5mg/mL.
5. the preparation method of magnetic ferroferric oxide/graphene composite material as claimed in claim 1 or 2, it is characterised in that：Water
The mass percent for closing hydrazine solution is 40 ~ 80%；Graphite oxide dispersion is 8 with the volume ratio of hydrazine hydrate solution:1~9:1.
6. the preparation method of magnetic ferroferric oxide/graphene composite material as claimed in claim 1 or 2, it is characterised in that：It is dry
Dry be vacuum dried at 60 ~ 70 DEG C.
7. magnetic ferroferric oxide/graphene composite material that prepared by method as claimed in claim 1 is in magnetic paint is prepared
Application.
8. application of the magnetic ferroferric oxide/graphene composite material as claimed in claim 7 in magnetic paint is prepared, it is special
Levy and be：Magnetic ferroferric oxide/graphene composite material is added in ethanol with 1 ~ 1.5mg/mL, ultrasonic disperse 10 ~
15min；Varnish is added, fully shaking, solution is layered, and abandoning supernatant continuously adds varnish, until solution is not stratified, obtains
To magnetic paint.
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| CN111749028A (en) * | 2020-07-07 | 2020-10-09 | 苏州康丽达精密电子有限公司 | Multilayer composite graphene electromagnetic shielding material and preparation method thereof |
| CN113861798A (en) * | 2021-09-28 | 2021-12-31 | 江门市翰尔威新材料有限公司 | Water-based paint with paint film capable of being adsorbed by magnet and preparation method thereof |
| CN115368801A (en) * | 2021-05-18 | 2022-11-22 | 江苏科辉环境科技有限公司 | Magnetized graphene coating and preparation method thereof |
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| CN113861798A (en) * | 2021-09-28 | 2021-12-31 | 江门市翰尔威新材料有限公司 | Water-based paint with paint film capable of being adsorbed by magnet and preparation method thereof |
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