CN107225237A - A kind of graphene is modified the preparation method and application of zinc powder - Google Patents
A kind of graphene is modified the preparation method and application of zinc powder Download PDFInfo
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- CN107225237A CN107225237A CN201710475595.XA CN201710475595A CN107225237A CN 107225237 A CN107225237 A CN 107225237A CN 201710475595 A CN201710475595 A CN 201710475595A CN 107225237 A CN107225237 A CN 107225237A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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Abstract
The invention provides the preparation method that a kind of graphene is modified zinc powder, comprise the following steps, first by after graphene solution and zinc powder uniformly mixing, obtain mixture；Then mixture above-mentioned steps obtained obtains the modification zinc powder of the dispersed graphene in surface after rotary evaporation.The present invention is using the processing mode of revolving, and by the dispersed encapsulated of graphene uniform on zinc powder surface, obtaining being capable of uniformly graphene coated zinc powder, i.e., the modification zinc powder of dispersed graphite alkenes material.Not only fundamentally solve graphite alkenes material and mix uneven disadvantage in the solution, it ensure that the dispersed of graphite alkenes material, and graphene is coated on zinc powder surface, it can ensure that its flat presentation of graphene reduces fold, preferably play its performance, so as to which the zinc powder after processing be added in practical application, it is ensured that the perfect performance of its premium properties.
Description
Technical field
The invention belongs to carbon material technical field, it is related to the preparation method that a kind of graphene is modified zinc powder, more particularly to one
Plant the method in zinc powder Dispersion on surface graphite alkenes material.
Background technology
Graphene (Graphene) is a kind of new material for the individual layer laminated structure being made up of carbon atom.It is one kind by carbon
Atom constitutes the flat film that hexangle type is in honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness with sp2 hybridized orbits.
As a kind of two dimensional crystal for the only one layer of atomic thickness being made up of carbon atom, it is current into most thin in application field
Material and most tough material, 200 times more taller than steel of fracture strength also have elasticity well, and stretch range can reach certainly
The 20% of body size；Graphene has huge theoretical specific surface area simultaneously, and physicochemical properties are stable, can be in high working voltage
With good structural stability is kept under high current fast charging and discharging, meanwhile, graphene also have excellent electric conductivity, can drop
Low internal resistance, improves the cyclical stability of ultracapacitor；And if graphene can manufacture ultra micro transistor npn npn, for producing
Following supercomputer.Replace silicon with graphene, the speed of service of computer processor will be fast hundreds times；In addition, graphite
Alkene is almost fully transparent, only absorbs 2.3% light.And it is very fine and close, even minimum gas atom (helium atom)
Also it can not penetrate.These features cause it to be highly suitable as the raw material of transparent electron product, such as transparent touch display screen, hair
Tabula rasa and solar panel.There is above-mentioned many excellent physical chemical property just because of graphene, its in energy storage material,
Environmental project, is widely used in terms of sensing sensitive, is referred to as " dark fund " or " king of new material ", and before potentially applying
Scape is vast, turns into global focus and study hotspot at present.
Such as paint field, from current anticorrosive paint market from the point of view of in the world, all material is every year because of corrosion loss about 1%
Weight, corrode the economic loss brought and account for the 4% of national economy total amount, anti-corrosion present situation allows of no optimist, especially heavy antisepsis is applied
Material field, the high-end anticorrosive paint market space is huge.Explicitly pointed out in " 13 " planning, development function anticorrosive paint,
Such as low surface treatment paint, nanocomposite coatings, heatproof moisture-proof coating, polyaniline paint, graphene coating.Therefore, graphite
Alkene is modified anticorrosive paint as one of focus studied at this stage.Graphene is as a kind of high fine and close sheet shape material material, such as
It intact can be added in coating, shielding action well can be played, prevent the entrance of corrosive medium, improve anti-corrosion property energy.
But in actual applications, the problem of graphene also has many and restraining factors, graphene are easily reunited just
It is a major obstacle for restricting graphene research and application.Because graphene makes in the presence of stronger model ylid bloom action power each other
It can not stable dispersion in a solvent, it is scattered after also easily reunite again and be difficult to open together.According to reported literature, numerous studies
The dispersion effect of graphene is improved by way of adding different types of dispersant or modification, but can not equally realize stone
Black alkene it is dispersed, and can also additionally introduce other impurities, subsequent production is adversely affected and processing cost increasing
Plus, and graphene with other materials when mixing, and is also easy to occur curling fold, this can directly affect graphene composite material
Effect in follow-up field.
Therefore, how to find a kind of method for being capable of dispersed graphene, solve the problem of graphene is easily reunited, into
For the downstream application field of graphene production firm and graphene major issue urgently to be resolved hurrily.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide the preparation method that a kind of graphene is modified zinc powder,
Particularly a kind of method in zinc powder Dispersion on surface graphite alkenes material, graphene prepared by the present invention is modified zinc powder can be effective
In zinc powder Dispersion on surface graphene, solve its easily reunite the problem of, be later stage graphene be modified zinc powder be more widely applied
Lay the foundation.
The invention provides the preparation method that a kind of graphene is modified zinc powder, comprise the following steps：
A) by after graphene solution and zinc powder uniformly mixing, mixture is obtained；
B) mixture for obtaining above-mentioned steps obtains the modified Zn of the dispersed graphene in surface after rotary evaporation
Powder.
It is preferred that, the mass ratio of the graphene and the zinc powder is (0.01~1)：100；
The zinc powder includes the one or more in zinc flake, spherical zinc powder and bar-shaped zinc powder.
It is preferred that, the graphene solution is the graphene solution after scattered；
The mass concentration of the graphene solution is 0.01%~20%.
It is preferred that, the size of the zinc powder is 1~5000 μm；
The graphene also includes the one or more in graphene oxide, redox graphene and modified graphene.
It is preferred that, the solvent of the graphene solution includes water, absolute ethyl alcohol, acetone, dimethylbenzene, n-butanol, methyl fourth
One or more in ketone, isopropanol and ethyl acetate.
It is preferred that, the step A) be specially：
Zinc powder is slowly added into the graphene solution after scattered, while uniform mixing, obtains mixture.
It is preferred that, the speed being slowly added to is 100~1000g/min；
The mixing includes stirring mixing；
The rotating speed of the stirring mixing is 200~1000rpm.
It is preferred that, the rotary speed of the rotary evaporation is 20~100rpm；
The temperature of the rotary evaporation is 40~90 DEG C；
The pressure of the rotary evaporation is less than or equal to 50KPa；
The time of the rotary evaporation is 0.5~5h.
It is preferred that, vacuum drying step is also included after the rotary evaporation；
The vacuum drying temperature is 30~90 DEG C；
The vacuum drying time is 0.5~8h；
The vacuum drying pressure is less than or equal to 80KPa.
Graphene prepared by above-mentioned technical proposal any one is modified application of the zinc powder in coating.
The invention provides the preparation method that a kind of graphene is modified zinc powder, comprise the following steps, it is first that graphene is molten
Liquid and zinc powder uniformly after mixing, obtain mixture；Then mixture above-mentioned steps obtained obtains table after rotary evaporation
The modification zinc powder of the dispersed graphene in face.Compared with prior art, the problem of present invention easily reunites for graphene, and show
The different degrees of presence of some preparation methods is reunited again, disperses inequality, introduces impurity, influence performance and raising processing cost
Defect.The processing mode using revolving of the invention, by the dispersed encapsulated of graphene uniform on zinc powder surface, can be obtained
To being capable of uniformly graphene coated zinc powder, i.e., the modification zinc powder of dispersed graphite alkenes material.Not only fundamentally solve
Graphite alkenes material mixes uneven disadvantage in the solution, ensure that the dispersed of graphite alkenes material, and by stone
Black alkene is coated on zinc powder surface, it is ensured that its flat presentation of graphene reduces fold, preferably plays its performance, so that will place
Zinc powder after reason is added in practical application, and graphene dispersion can be solved the problems, such as well, it is ensured that the perfection of its premium properties
Play.
Test result indicates that, the preparation method that the present invention is provided can realize graphene being uniformly distributed on zinc powder surface,
Graphite alkenes material modification zinc powder is uniformly added in coating, can prepare low thickness, high intensity, for a long time it is corrosion-resistant,
The new coating of low cost.
Brief description of the drawings
Fig. 1 is the FESEM microscopic appearance figures of modification piece shape zinc powder section prepared by the embodiment of the present invention 1；
Fig. 2 is the Raman spectrogram of modified spherical zinc powder prepared by the embodiment of the present invention 1；
Fig. 3 is the cross-section structure of the coating containing common zinc powder prepared by the embodiment of the present invention 3；
Fig. 4 is the cross-section structure of the coating that zinc powder is modified containing graphene prepared by the embodiment of the present invention 3.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are intended merely to further illustrate the features and advantages of the present invention, rather than to invention claim
Limitation.
All raw materials of the present invention, originate to it and are not particularly limited, commercially buying or according to people in the art
Known to member prepared by conventional method.
All raw materials of the present invention, its purity is not particularly limited, compound present invention preferably employs pure or graphene is analyzed
The conventional purity that Material Field is used.
The invention provides the preparation method that a kind of graphene is modified zinc powder, it is characterised in that comprises the following steps：
A) by after graphene solution and zinc powder uniformly mixing, mixture is obtained；
B) mixture for obtaining above-mentioned steps obtains the modified Zn of the dispersed graphene in surface after rotary evaporation
Powder.
The specific pattern of the zinc powder is not particularly limited the present invention, with Zinc Particles Morphology well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, this
Invent the zinc powder and preferably include one or more in zinc flake, spherical zinc powder and bar-shaped zinc powder, more preferably sheet zinc
Powder, spherical zinc powder or bar-shaped zinc powder.
The size of the zinc powder is not particularly limited the present invention, and the size with zinc powder well known to those skilled in the art is
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product requirement and quality requirement
The size (particle diameter, piece footpath or size) of the bright zinc powder is preferably 1~5000 μm, more preferably 10~3000 μm, more preferably
50~1000 μm, most preferably 100~500 μm.
The specifically chosen of the zinc powder is not particularly limited the present invention, is with zinc powder well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product requirement and quality requirement
The bright zinc powder preferably includes zinc powder and/or the powdered granule of other zinc compounds, such as Zinc oxide particles.
Definition of the present invention to the graphene is not particularly limited, with the general of graphene well known to those skilled in the art
Thought, those skilled in the art can be selected and be adjusted according to practical situations, product requirement and quality requirement,
Graphene of the present invention is preferably the graphene of broad sense, i.e. graphite alkenes material, preferably includes narrow sense graphene, graphite oxide
One or more in alkene, redox graphene and modified graphene, more preferably single-layer graphene, multi-layer graphene, oxygen
Graphite alkene, redox graphene or modified graphene, most preferably single-layer graphene, multi-layer graphene or graphite oxide
Alkene.
Specifically, graphene of the present invention can include the graphite alkenes material of a variety of types commercially available on the market, specifically
High-quality graphene (the patent No. that preferably Ou Bo companies produce：CN 106082198A), the graphene oxide (patent No.：CN
106115669A) with the one or more in graphene oxide (CN 106430175A).
The concentration of the graphene solution is not particularly limited the present invention, with graphene well known to those skilled in the art
The concentration of solution, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
Select and adjust, the concentration of graphene solution of the present invention is preferably 0.01%~20%, more preferably 0.05%~5%, most
Preferably 0.1%~1%.
The solvent of the graphene solution is not particularly limited the present invention, is used for stone with well known to those skilled in the art
The Conventional solvents of black alkene solution, those skilled in the art can want according to practical condition, product requirement and quality
Ask and selected and adjusted, the solvent of graphene solution of the present invention is preferably water, absolute ethyl alcohol, acetone, dimethylbenzene, positive fourth
One or more in alcohol, espeleton, isopropanol and ethyl acetate, more preferably water, absolute ethyl alcohol, acetone, dimethylbenzene, just
Butanol, espeleton, isopropanol or ethyl acetate, more preferably water, absolute ethyl alcohol, acetone or dimethylbenzene.
The present invention is improves the dispersion effect of follow-up graphene, and the graphene solution is preferably the graphite after scattered
Alkene solution.The preparation method of the graphene solution is not particularly limited the present invention, with system well known to those skilled in the art
Preparation Method, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, scattered preferably ultrasonic agitation processing of the present invention.
The consumption of the graphene solution and zinc powder is not particularly limited the present invention, with well known to those skilled in the art
Conventional ratio, those skilled in the art can be selected according to practical condition, product requirement and quality requirement
And adjustment, the mass ratio of graphene of the present invention and the zinc powder is preferably (0.01~1)：100, more preferably (0.05~
0.8)：100, more preferably (0.08~0.7)：100, be most preferably (0.1~0.5)：100, it is specifically as follows (0.2~0.4)：
100。
The detailed process of the mixing is not particularly limited the present invention, with mixed process well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, with
Uniformly it is mixed into preferred scheme, the specific steps of mixing of the present invention, i.e. step A) it is particularly preferred as：
Zinc powder is slowly added into the graphene solution after scattered, while uniform mixing, obtains mixture.
The design parameter being slowly added to is not particularly limited the present invention, with well known to those skilled in the art slow
The addition speed of addition, those skilled in the art can enter according to practical condition, product requirement and quality requirement
Row selection and adjustment, the speed of the present invention being slowly added to is preferably 100~1000g/min, more preferably 200~900g/
Min, more preferably 400~700g/min, more preferably 500~600g/min, most preferably 300~500g/min.
The mode of the mixing is not particularly limited the present invention, is with hybrid mode well known to those skilled in the art
Can, those skilled in the art can be selected and be adjusted, this hair according to practical condition, product requirement and quality requirement
The bright mixing preferably includes stirring mixing.
The design parameter of the stirring mixing is not particularly limited the present invention, with mixing well known to those skilled in the art
Parameter, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the rotating speed of stirring mixing of the present invention is preferably 200~1000rpm, more preferably 300~900rpm, more preferably
400~800rpm, more preferably 500~700rpm, most preferably 350~500rpm.
The mixture that then present invention obtains above-mentioned steps obtains the dispersed graphene in surface after rotary evaporation
Modification zinc powder.
The rotating speed of the rotary evaporation is not particularly limited the present invention, with rotary evaporation well known to those skilled in the art
Rotating speed, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the rotation is steamed
The rotary speed of hair is preferably 20~100rpm, more preferably 30~90rpm, more preferably 40~80rpm, most preferably 40~
60rpm, or 50~70rpm.
The temperature of the rotary evaporation is not particularly limited the present invention, with rotary evaporation well known to those skilled in the art
Temperature, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the rotation is steamed
The temperature of hair is preferably 40~90 DEG C, more preferably 50~80 DEG C, more preferably 60~70 DEG C, most preferably 60~75 DEG C.
The time of the rotary evaporation is not particularly limited the present invention, with rotary evaporation well known to those skilled in the art
Time, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the rotation is steamed
The time of hair is preferably 0.5~5h, more preferably 1~4.5h, more preferably 1.5~4h, most preferably 2~3.5h, specifically may be used
Think, loosely powdered is finally presented with the compound zinc powder by graphene.
The pressure of the rotary evaporation is not particularly limited the present invention, with rotary evaporation well known to those skilled in the art
Pressure, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the rotation is steamed
The pressure of hair is preferably smaller than equal to 50KPa, more preferably less than or equal to more preferably less than or equal to 40KPa, 30KPa, is specifically as follows
10~50KPa, is either 10~40KPa or is 10~29KPa.
The equipment of the rotary evaporation is not particularly limited the present invention, and those skilled in the art can be according to actual production
Situation, product requirement and quality requirement are selected and adjusted, and the equipment of rotary evaporation of the present invention is preferably that revolving is steamed
Send out device.
The present invention optimizes and complete process route to improve the practicality and performance of modified zinc powder, after the rotary evaporation
It is preferred that also including drying steps.
The concrete mode of the drying is not particularly limited the present invention, with drying mode well known to those skilled in the art
, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement, this
It is preferably vacuum drying to invent the drying.
The vacuum drying temperature is not particularly limited the present invention, with vacuum drying well known to those skilled in the art
Temperature, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the vacuum is done
Dry temperature is preferably 30~90 DEG C, more preferably 40~80 DEG C, most preferably 50~80 DEG C, most preferably 60~75 DEG C.
The vacuum drying time is not particularly limited the present invention, with vacuum drying well known to those skilled in the art
Time, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the vacuum is done
The dry time is preferably 0.5~8h, more preferably 1~7h, more preferably 2~6.5h, most preferably 3~5h.
The vacuum drying pressure is not particularly limited the present invention, with vacuum drying well known to those skilled in the art
Pressure, those skilled in the art can be selected according to practical condition, product requirement and quality requirement and
Adjustment, the present invention improves the dispersing uniformity of graphene for preferably graphene and zinc powder are combined closely, and the vacuum is done
Dry pressure is preferably smaller than equal to 80KPa, more preferably less than or equal to 60KPa, or 10~60KPa, more preferably less than or equal to
40KPa, or 20~40KPa.
The present invention uses rotary evaporation technique, by controlling vacuum, rotary speed, revolving temperature (bath temperature) etc. to make
Graphene uniform is coated in zinc powder surface, untill material is in drying regime, so that by graphene, macroscopical or micron-sized zinc powder
It is closely linked, can effectively solves graphene dispersion problem of non-uniform, preferably plays its premium properties, but also
The zinc powder material of grapheme material can be obtain a uniformly coated, dispersed coating of the graphene to zinc powder is turned into existing initiatively
It is real.And the present invention is special under conditions of existing without protective gas, carries out aforesaid operations, so that the production stream simplified
Journey, production equipment and reduce production consumption.Preparation method technique that the present invention is provided is simple, mild condition, safety and environmental protection,
It is more suitable for the big production of technology.
Above-mentioned steps of the present invention have obtained the modification zinc powder of the dispersed graphene in surface, and the present invention is to the scattered stone
The thickness of black alkene is not particularly limited, and those skilled in the art can want according to practical situations, product requirement and quality
Ask and selected and adjusted, to realize that grapheme material is dispersed for preferred scheme, scattered graphene layer of the present invention
Thickness control is at 0.01~10 μm, and preferred thickness can be regulated and controled according to the actual requirements, more specifically preferably 0.01~10 μm, more
Preferably 0.061~10 μm, more preferably 0.1~5 μm, more preferably more preferably 0.5~3 μm, 1~2 μm.
The processing mode using revolving of the invention, can by the dispersed encapsulated of graphene uniform on zinc powder surface
Obtain the graphene zinc powder that can uniformly coat, i.e., dispersed graphene.Graphene is not only fundamentally solved in solution
The uneven disadvantage of middle mixing, ensure that the dispersed of graphene, and graphene is coated on into particle surface, Ke Yibao
Its flat presentation for demonstrate,proving graphene reduces fold, its performance is preferably played, so that the particle after processing is added into practical application
In, graphene dispersion can be solved the problems, such as well, it is ensured that the perfect performance of its premium properties.
Zinc powder answering in coating is modified present invention also offers the graphene prepared by above-mentioned technical proposal any one
With.The specifically chosen of the coating is not particularly limited the present invention, contains spelter coating with well known to those skilled in the art,
Those skilled in the art can be selected and be adjusted according to practical situations, product requirement and quality requirement, the present invention
The coating preferably include epoxy zinc-enriched paint, zinc powder powdery paints, inorganic zinc coatings and one kind in Dacroment masking liquid or
It is a variety of.
Above-mentioned steps of the present invention provide the preparation method that a kind of graphene is modified zinc powder, and the present invention uses rotary evaporation
Method, by controlling the vacuum of revolving process, rotary speed, revolving temperature (bath temperature) etc. to be coated in graphene uniform
Zinc powder surface, untill material is in drying regime, so that graphene, macroscopical or micron-sized zinc powder are closely linked,
Dispersed graphene has been obtained, and graphene has been closely linked with macroscopical or micron-sized zinc powder；Effective solution
Certainly graphene mixes uneven disadvantage in the solution, and graphene disperses uneven in containing macroscopical or microcosmic zinc powder material
The problem of, dispersant etc. will not also be introduced other mixed and disorderly materials, preferably play the premium properties of grapheme material, but also
The zinc powder material of grapheme material can be obtain a uniformly coated, coating of the graphene to zinc powder is become a reality initiatively, and be
Later stage graphene, which is more widely applied, to lay the foundation.
Test result indicates that, the preparation method that the present invention is provided can realize graphene being uniformly distributed on zinc powder surface,
Graphite alkenes material modification zinc powder is uniformly added in coating, can prepare low thickness, high intensity, for a long time it is corrosion-resistant,
The new coating of low cost.
In order to further illustrate the present invention, zinc powder is modified to a kind of graphene that the present invention is provided with reference to embodiments
Preparation method is described in detail, but it is to be understood that these embodiments are carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, simply to further illustrate the features and advantages of the present invention,
Rather than limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following embodiments.
Embodiment 1
1) it is 0.5% graphene oxide (CN 106115669A) aqueous solution, ultrasonic agitation 3h to take a certain amount of content；
2) 500g piece shape zinc powders are added slowly to step 1 under mechanical stirring according to 0.5% ratio) in obtained graphite
In alkene solution, 30min is persistently stirred；
3) by step 2) gained mixed solution be added in rotary evaporator；
4) it is 0.09Mpa to control vacuum, and 80 DEG C of bath temperature, rotary speed 60RPM is lasting to carry out, to material in dry
Untill dry state, the zinc powder of the dispersed graphene in surface, i.e. graphene coating particles are obtained.
5) embedding, microtomy are passed through to the product of preparation.
Product prepared by the embodiment of the present invention 1 is characterized and analyzed by field emission scanning electron microscope.
Referring to Fig. 1, Fig. 1 is the FESEM microscopic appearance figures of modification piece shape zinc powder section prepared by the embodiment of the present invention 1.By
Fig. 1 is it can be found that there is one layer of obvious film in zinc powder slice surface, and thickness about 61nm illustrates the painting that graphene can be complete
Overlay on zinc powder surface.
Embodiment 2
1) it is 0.3% modified graphene ethanol solution, ultrasonic agitation 3h to take 1000g contents；
2) the spherical zinc powders of 500g are added slowly to step 1 under mechanical stirring according to 0.5% ratio) in obtained graphite
In alkene solution, 30min is persistently stirred；
3) by step 2) gained mixed solution be added in rotary evaporator；
4) it is 0.09Mpa to control vacuum, and 60 DEG C of bath temperature, rotary speed 60RPM is lasting to carry out, to material in dry
Untill dry state, the zinc powder of the dispersed graphene in surface, i.e. graphene coating particles are obtained.
Raman phenetic analysis is carried out to product prepared by the embodiment of the present invention 2.
Referring to Fig. 2, Fig. 2 is the Raman spectrogram of modified spherical zinc powder prepared by the embodiment of the present invention 1.
Distribution situation of the graphene on zinc powder surface, red area can clearly be told by the Raman spectrogram in Fig. 2
There is the characteristic peak of graphene, blue region there is no the characteristic peak of graphene, i.e. red area to exist for graphene, and blue region is
Spherical zinc powder.
Embodiment 3
1) it is 0.3% graphene oxide (CN 106115669A) aqueous solution, ultrasonic agitation 3h to take 1000g contents；
2) the spherical zinc powders of 500g are added slowly to step 1 under mechanical stirring according to 0.5% ratio) in obtained graphite
In alkene solution, 30min is persistently stirred；
3) by step 2) gained mixed solution be added in rotary evaporator；
4) it is 0.09Mpa to control vacuum, and 80 DEG C of bath temperature, rotary speed 60RPM is lasting to carry out, to material in dry
Untill dry state, the zinc powder of the dispersed graphene in surface, i.e. graphene coating particles are obtained；
5) raw material such as modified zinc powder and epoxy resin, dimethylbenzene is mixed, prepares epoxy zinc powder coating；
6) according to the preparation method of step 5, modified zinc powder is substituted with the common zinc powder of same size, the painting of epoxy zinc powder is prepared
Material；
The coating containing common zinc powder and the coating containing graphene modification zinc powder prepared to the embodiment of the present invention is for sample
Plate is conserved after the same terms, carries out fractograph analysis.
Referring to Fig. 3, Fig. 3 is the cross-section structure of the coating containing common zinc powder prepared by the embodiment of the present invention 3.Referring to figure
4, Fig. 4 be the cross-section structure of the coating that zinc powder is modified containing graphene prepared by the embodiment of the present invention 3.
Contrasted, the morphology analysis of two kinds of coating sections, section is uneven before modified, existed substantially from Fig. 3 and Fig. 4
Hole；The modified flat state of section, there is no pore structure.This shows that the latter has stronger anti-corrosion property than the former
Energy.
Hole is to influence the hole in the key factor of coating property, coating that the corrosive medium in the external world is readily able to
Corrosion is caused through paint film contact matrix surface.Therefore, the coating of same system, compact in paint film degree is higher, then erosion resistance is got over
By force.
Detailed Jie has been carried out to a kind of method in zinc powder Dispersion on surface graphite alkenes material that the present invention is provided above
Continue, specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example is only
It is to be used to help understand method and its core concept of the invention, including best mode, and also causes any skill of this area
Art personnel can put into practice the present invention, including manufacture and the method using any device or system, and any combination of implementation.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, can also be to this hair
Bright to carry out some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.It is of the invention special
Profit protection scope be defined by the claims, and may include those skilled in the art it is conceivable that other embodiment.Such as
Really these other embodiments have the structural element for being not different from claim character express, or if they include and power
Equivalent structural elements of the character express without essence difference that profit is required, then these other embodiments should also be included in claim
In the range of.
Claims (10)
1. a kind of graphene is modified the preparation method of zinc powder, it is characterised in that comprise the following steps：
A) by after graphene solution and zinc powder uniformly mixing, mixture is obtained；
B) mixture for obtaining above-mentioned steps obtains the modification zinc powder of the dispersed graphene in surface after rotary evaporation.
2. preparation method according to claim 1, it is characterised in that the mass ratio of the graphene and the zinc powder is
(0.01~1)：100；
The zinc powder includes the one or more in zinc flake, spherical zinc powder and bar-shaped zinc powder.
3. preparation method according to claim 1, it is characterised in that the graphene solution is the graphite after scattered
Alkene solution；
The mass concentration of the graphene solution is 0.01%~20%.
4. preparation method according to claim 1, it is characterised in that the size of the zinc powder is 1~5000 μm；
The graphene also includes the one or more in graphene oxide, redox graphene and modified graphene.
5. preparation method according to claim 1, it is characterised in that the solvent of the graphene solution includes water, anhydrous
One or more in ethanol, acetone, dimethylbenzene, n-butanol, espeleton, isopropanol and ethyl acetate.
6. preparation method according to claim 1, it is characterised in that the step A) be specially：
Zinc powder is slowly added into the graphene solution after scattered, while uniform mixing, obtains mixture.
7. preparation method according to claim 6, it is characterised in that the speed being slowly added to is 100~1000g/
min；
The mixing includes stirring mixing；
The rotating speed of the stirring mixing is 200~1000rpm.
8. the preparation method according to claim 1~7 any one, it is characterised in that the rotation speed of the rotary evaporation
Spend for 20~100rpm；
The temperature of the rotary evaporation is 40~90 DEG C；
The pressure of the rotary evaporation is less than or equal to 50KPa；
The time of the rotary evaporation is 0.5~5h.
9. the preparation method according to claim 1~7 any one, it is characterised in that also include after the rotary evaporation
Vacuum drying step；
The vacuum drying temperature is 30~90 DEG C；
The vacuum drying time is 0.5~8h；
The vacuum drying pressure is less than or equal to 80KPa.
10. the graphene prepared by claim 1~9 any one is modified application of the zinc powder in coating.
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| CN111793373A (en) * | 2020-07-31 | 2020-10-20 | 株洲飞鹿高新材料技术股份有限公司 | Preparation method of modified graphene slurry, epoxy anticorrosive primer and preparation method thereof |
| CN112592611A (en) * | 2021-03-02 | 2021-04-02 | 广东合胜实业股份有限公司 | Graphene-based modified antibacterial and antiviral coating and preparation method thereof |
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