CN107163775A - A kind of resin anti-corrosive paint containing graphene/ferric oxide composite material and preparation method thereof - Google Patents
A kind of resin anti-corrosive paint containing graphene/ferric oxide composite material and preparation method thereof Download PDFInfo
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- CN107163775A CN107163775A CN201710292940.6A CN201710292940A CN107163775A CN 107163775 A CN107163775 A CN 107163775A CN 201710292940 A CN201710292940 A CN 201710292940A CN 107163775 A CN107163775 A CN 107163775A
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- Prior art keywords
- graphene
- resin
- present
- iron trioxide
- rotary evaporation
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Classifications
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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
Abstract
The invention provides a kind of resin anti-corrosive paint, including, resin, the composite of graphene and di-iron trioxide, auxiliary agent and solvent.The present invention changes the addition manner of graphite alkenes material, di-iron trioxide in graphene and coating is combined first, obtain the composite of graphene and di-iron trioxide, then the graphene and the composite particles of di-iron trioxide after processing are combined with other compositions, obtain resin anti-corrosive paint, graphene dispersion can be solved the problems, such as well, ensure the perfect performance of its premium properties, and other auxiliary agents need not be added, reduce the introducing of impurity, solve graphite alkenes material and uneven disadvantage is mixed in coating system, it ensure that the dispersed of graphene, while the composite of graphene and di-iron trioxide, it can ensure that its flat presentation of graphene reduces fold, preferably play its performance.
Description
Technical field
The invention belongs to anticorrosive paint technology field, it is related to a kind of resin anti-corrosive paint and preparation method thereof, more particularly to
A kind of resin anti-corrosive paint containing graphene/ferric oxide composite material and preparation method thereof.
Background technology
Graphene (Graphene) is a kind of new material for the individual layer laminated structure being made up of carbon atom, as one kind by carbon
The two dimensional crystal of former molecular only one layer of atomic thickness, it is current to enter material most thin in application field and most tough
Material, 200 times more taller than steel of fracture strength also has elasticity well, stretch range can reach the 20% of own dimensions；
Meanwhile, graphene also has excellent electric conductivity, can reduce internal resistance, improves the cyclical stability of ultracapacitor；In addition, stone
Black alkene is almost fully transparent, only absorbs 2.3% light, and very fine and close, even (helium is former for minimum gas atom
Son) it can not also penetrate.These features cause it to be highly suitable for a variety of subjects and field, also have just because of graphene upper
Many excellent physical chemical property are stated, it is widely used, be referred to as at energy storage material, environmental project, sensing sensitive aspect
" dark fund " or " king of new material ", and potential application prospect is vast, has turned into global focus at present with grinding
Study carefully focus, while also having moved towards industrialization from conceptual phase on derivatives such as graphenes, cause the extensive ginseng of all trades and professions
With.
At present, the derivative such as graphene or graphene oxide, i.e. graphite alkenes material, can be used as preferably addition material
Material, imparts the new feature of composite, has expanded the application field of graphene composite material.Such as graphene or oxidation stone
Black alkene is applied in coating Related product, it is possible to achieve the mutual supplement with each other's advantages and reinforcement of two kinds of materials, significantly lifts coating products
Performance.And from world wide, all material because of the weight of corrosion loss about 1%, corrodes the economy brought every year
Loss accounts for the 4% of national economy total amount, and this loss is even more serious in the torrid zone and marine environment, such as current China only ocean
Corrode the loss brought with regard to the 3% of super GDP, anti-corrosion road is shouldered heavy responsibilities.Make a general survey of the country, the positive strength of the Belt and Road east wind, " 13
Five " planning go up on the stage and make a theatrical pose, while the industry fast development such as ocean engineering, shipbuilding and green marine wind energy, industrial antisepsis is applied
Material and field of coating enter the gold period of fast growth, and its market scale has been only second to building in various coating varieties
Coating and occupy second.In recent years, China is in infrastructure construction, cities and towns My Perspective On The Co-building and new countryside construction, the Olympic Games,
Shanghai etc. is settled in the Asian Games, the maximum Disneyland of Shanghai World's Fair and the whole world, huge coating demand is suffered from, new
International situation and national policy under, provide new opportunity for the fast development of coating industry and industrial antisepsis coating, send out energetically
New anti-corrosion coating is opened up, is had broad prospects and realistic meaning.
In recent years, the coating products containing graphite alkenes material gradually have relevant report, but in actual applications, stone
The problem of black alkene also has many and restraining factors, such as graphene are easily reunited.Because graphene and its derivative compare surface
Product is larger, there is stronger model ylid bloom action power each other, reunites with wrapping phenomena substantially, prevents it from stable dispersion, disperses
Also easily reunite again afterwards and be difficult to open together.Although having numerous studies by adding different types of dispersant or modification
Mode improve the dispersion effect of graphene, but effect is poor in practical application, and can also additionally introduce other impurities, right
Follow-up study is adversely affected, and when being mixed with hard material, is also easy to occur curling fold, these are all by direct shadow
The effect that phonolite ink alkenes material can be played.
Therefore, a kind of graphene/ferric oxide composite material how is obtained so that graphene can be in coating system
Preferably distribution, is to influence the key factor of coating property, is also that many application vendors and a line research staff are urgently to be resolved hurrily
Problem.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of graphene/ferric oxide composite material
And preparation method thereof, graphene/ferric oxide composite material that the present invention is provided, graphene can be dispersed, composite wood
Graphene has preferable its flat presentation, less fold, so that with better performance in material.
The invention provides a kind of resin anti-corrosive paint, including, resin, the composite of graphene and di-iron trioxide,
Auxiliary agent and solvent.
It is preferred that, the resin is 25~55 parts by weight；
The composite of graphene and di-iron trioxide is 35~65 parts by weight；
Auxiliary agent is 17~32 parts by weight；
Solvent is 103~143 parts by weight；
The auxiliary agent includes the one or more in curing agent, accelerator, anti-settling agent, defoamer and filler.
It is preferred that, the curing agent is 1.5~3.5 parts by weight；
The accelerator is 0.05~0.2 parts by weight；
The anti-settling agent is 2.4~4.5 parts by weight；
The defoamer is 0.5~1.5 parts by weight；
The filler is 12.3~22.3 parts by weight.
It is preferred that, the composite of the graphene and di-iron trioxide aoxidizes two for the three of the uniform composite graphite alkene in surface
Iron material；
The graphene includes the one or more in graphene oxide, graphene and modified graphene；
The resin is included in epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin
It is one or more；
The solvent includes water, acetone, ethanol, isopropanol, butanone, 2-Pyrrolidone, dimethylbenzene, n-butanol, carbonic acid third
One or more in alkene ester, propylene glycol monomethyl ether and butyl acetate；
The defoamer include organosiloxane defoamer, polyether antifoam agent and one kind in dimethicone defoamer or
It is a variety of；
The anti-settling agent includes anti-settling agent 3300, organic clay, organic pottery clay, aerosil, Tissuemat E and fibre
One or more in the plain ether of dimension；
The curing agent includes polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, polyethylene polyamine and polyethers two
One or more in amine.
Present invention also offers a kind of preparation method of resin anti-corrosive paint, comprise the following steps：
A graphene and di-iron trioxide) are obtained into the composite wood of graphene and di-iron trioxide after first mixing
Material；
B graphene and the composite of di-iron trioxide, resin and the solvent for) obtaining above-mentioned steps are mixed, warp
Cross after rotary evaporation again, obtain mixture；
C after the mixture and auxiliary agent for) obtaining above-mentioned steps are mixed again, resin anti-corrosive paint is obtained.
It is preferred that, the step A) be specially：
A1) by after graphene solution and di-iron trioxide uniformly mixing, mixture is obtained；
A2) mixture for obtaining above-mentioned steps obtains the graphite of the dispersed graphene in surface after rotary evaporation
Alkene and ferric oxide composite material.
It is preferred that, the mass ratio of the graphene and the di-iron trioxide is (0.01~1)：100；
The step A1) in, the rotary speed of the rotary evaporation is 40~70rpm；
The temperature of the rotary evaporation is 60~80 DEG C；
The pressure of the rotary evaporation is 0.003~0.05MPa；
The time of the rotary evaporation is 0.5~2h.
It is preferred that, the step B) in, the rotary speed of the rotary evaporation again is 40~70rpm；
The temperature of the rotary evaporation again is 60~80 DEG C；
The pressure of the rotary evaporation again is 0.003~0.05MPa；
The time of the rotary evaporation again is 0.5~2h.
It is preferred that, the step C) be specially：
C1 mixture, filler, anti-settling agent and the defoamer for) obtaining above-mentioned steps obtain resin after stirring mixing
The first component of anticorrosive paint；
By curing agent, accelerator and solvent after being again stirring for mixing, the second component of resin anti-corrosive paint is obtained；
The auxiliary agent includes the one or more in curing agent, accelerator, anti-settling agent, defoamer and filler.
It is preferred that, the rotating speed of the stirring mixing is 1000~2000rpm；The time of the stirring mixing is small for 1~3
When；
The rotating speed for being again stirring for mixing is 1000~1500rpm；The time for being again stirring for mixing is 0.5~2
Hour.
The invention provides a kind of resin anti-corrosive paint, including, resin, the composite of graphene and di-iron trioxide,
Auxiliary agent and solvent.Compared with prior art, the problem of present invention easily reunites for graphene, and existing process for dispersing is different
The presence of degree is reunited again, disperses inequality, introduces impurity, influence performance and the defect for improving processing cost.And in reality
Border is applied to during coating, it is found that directly mixing or addition dispersant are unable to solve graphene agglomeration traits, it is difficult to protect
Card is dispersed and flexible, is also easy to introduce impurity, and then causes that anticorrosive paint salt-fog resistant time is short, shock resistance
The many defects of difference and film layer thickness etc..The addition manner for changing graphite alkenes material of the invention, first by stone
The composite that hard material -- di-iron trioxide is combined, graphene and di-iron trioxide is obtained in black alkene and coating,
Then the graphene and the composite particles of di-iron trioxide after processing are combined with other compositions, obtains resin anti-corrosive paint, energy
It is enough to solve the problems, such as graphene dispersion well, it is ensured that the perfect performance of its premium properties, and other auxiliary agents need not be added, subtract
The introducing of impurity is lacked, has fundamentally solved soft graphite alkenes material and uneven disadvantage, energy are mixed in coating system
Enough ensure the dispersed of graphene, while the composite of graphene and di-iron trioxide, it is ensured that the tiling of graphene
State reduces fold, preferably plays its performance.
Test result indicates that, the preparation method cost that the present invention is provided is low, can solve graphene and be mixed in coating system
The uneven disadvantage easily reunited is closed, the dispersed of graphite alkenes material is ensure that, it is less with preferable its flat presentation
Fold；And prepare coating cost is low, good impact resistance, high hardness, corrosion-resistant time overlength and environment-friendly.
Brief description of the drawings
Fig. 1 is the SEM scannings of graphene/ferric oxide composite material microscopic appearance prepared by the embodiment of the present invention 1
Electromicroscopic photograph；
Fig. 2 is the SEM stereoscan photographs of common ferric oxide particle microscopic appearance；
Fig. 3 is the polarization of resin anti-corrosive paint prepared by the embodiment of the present invention 1 and the common anticorrosive paint containing di-iron trioxide
Curve comparison figure.
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, and present invention preferably employs analyze pure or composite neck
The conventional purity that domain is used.
The invention provides a kind of resin anti-corrosive paint, including, resin, the composite of graphene and di-iron trioxide,
Auxiliary agent and solvent.
The resin is not particularly limited the present invention, is with resin types well known to those skilled in the art and model
Can, those skilled in the art can be selected and be adjusted, this hair according to practical situations, product requirement and quality requirement
The bright resin preferably includes one in epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin
Plant or a variety of, more preferably epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin or superchlorinated polyvinyl chloride resin, most preferably
For epoxy resin, acrylic resin or fluorocarbon resin.
The other specification of the resin is not particularly limited the present invention, with usual resins well known to those skilled in the art
Parameter, those skilled in the art can be selected according to practical situations, product requirement and quality requirement and
Adjustment.
The addition of the resin is not particularly limited the present invention, is applied with resin resistant well known to those skilled in the art
The proportioning of the usual resins of material, those skilled in the art can want according to practical situations, product requirement and quality
Ask and selected and adjusted, the addition of resin of the present invention is preferably 25~55 parts by weight, more preferably 30~50 weight
Part, most preferably 35~45 parts by weight.
The specifically chosen of the solvent is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
With solvent, those skilled in the art can be selected according to practical situations, product requirement and quality requirement and
Adjustment, solvent of the present invention preferably include water, acetone, ethanol, isopropanol, butanone, 2-Pyrrolidone, dimethylbenzene, n-butanol,
One or more in propene carbonate, propylene glycol monomethyl ether and butyl acetate, more preferably water, acetone, ethanol, isopropanol, fourth
Ketone, 2-Pyrrolidone, dimethylbenzene, n-butanol, propene carbonate, propylene glycol monomethyl ether or butyl acetate.
The addition of the solvent is not particularly limited the present invention, is applied with resin resistant well known to those skilled in the art
The proportioning of the Conventional solvents of material, those skilled in the art can want according to practical situations, product requirement and quality
Ask and selected and adjusted, the addition of solvent of the present invention is preferably 103~143 parts by weight, more preferably 113~133
Parts by weight, most preferably 118~128 parts by weight.
The present invention is widened and preferably also wrapped in application field, the anticorrosive paint to improve the practicality of resin anti-corrosive paint
Include auxiliary agent.
Total addition of the auxiliary agent is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
Conven-tional adjuvants proportioning, those skilled in the art can be according to practical situations, product requirement and quality requirement
Selected and adjusted, total addition of auxiliary agent of the present invention is preferably 17~32 parts by weight, more preferably 20~30 weight
Part, most preferably 22~28 parts by weight.
The species of the auxiliary agent is not particularly limited the present invention, with anticorrosive paint auxiliary agent 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, this
Invent the auxiliary agent and preferably include one or more in curing agent, accelerator, anti-settling agent, defoamer and filler, it is preferably solid
Two or more in agent, accelerator, anti-settling agent, defoamer and filler, or curing agent, accelerator, anti-settling agent, disappear
Infusion and filler.
The addition of the curing agent is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
Conventional solidified dose of proportioning, those skilled in the art can according to practical situations, product requirement and quality will
Ask and selected and adjusted, the addition of curing agent of the present invention is preferably 1.5~3.5 parts by weight, more preferably 1.5~
3.5 parts by weight, most preferably 1.5~3.5 parts by weight.
The specifically chosen of the curing agent is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art
Material curing agent, those skilled in the art can be selected according to practical situations, product requirement and quality requirement
Select and adjust, it is many that curing agent of the present invention preferably includes polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, many ethene
One or more in amine and polyether diamine, more preferably polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, many ethene
Polyamines or polyether diamine.
The addition of the accelerator is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
Conventional accelerator proportioning, those skilled in the art can according to practical situations, product requirement and quality will
Ask and selected and adjusted, the addition of accelerator of the present invention is preferably 0.05~0.2 parts by weight, more preferably 0.08~
0.18 parts by weight, most preferably 0.1~0.15 parts by weight.
The specifically chosen of the accelerator is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art
Material uses accelerator, and those skilled in the art can be selected according to practical situations, product requirement and quality requirement
Select and adjust, accelerator of the present invention preferably includes DMP-30.
The addition of the anti-settling agent is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
Conventional anti-settling agent proportioning, those skilled in the art can according to practical situations, product requirement and quality will
Ask and selected and adjusted, the addition of anti-settling agent of the present invention is preferably 2.4~4.5 parts by weight, more preferably 2.9~
4.0 parts by weight, most preferably 3.3~3.6 parts by weight.
The specifically chosen of the anti-settling agent is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art
Material anti-settling agent, those skilled in the art can be selected according to practical situations, product requirement and quality requirement
Select and adjust, anti-settling agent of the present invention preferably includes anti-settling agent 3300, organic clay, organic pottery clay, aerosil, poly-
One or more in ethylene waxes and cellulose ether, more preferably anti-settling agent 3300, organic clay, organic pottery clay, gas phase dioxy
Two or more in SiClx, Tissuemat E and cellulose ether, are most preferably (Mo Nuolong) MONORAL3300 and organic pottery clay.
The addition of the defoamer is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
Conventional antifoam proportioning, those skilled in the art can according to practical situations, product requirement and quality will
Ask and selected and adjusted, the addition of defoamer of the present invention is preferably 0.5~1.5 parts by weight, more preferably 0.7~
1.3 parts by weight, most preferably 0.9~1.1 parts by weight.
The specifically chosen of the defoamer is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art
Material defoamer, those skilled in the art can be selected according to practical situations, product requirement and quality requirement
Select and adjust, defoamer of the present invention preferably includes organosiloxane defoamer, polyether antifoam agent and dimethicone froth breaking
One or more in agent, more preferably organosiloxane defoamer, polyether antifoam agent or dimethicone defoamer.
The addition of the filler is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
The proportioning of conventional fillers, those skilled in the art can enter according to practical situations, product requirement and quality requirement
Row selection and adjustment, the addition of filler of the present invention is preferably 12.3~22.3 parts by weight, more preferably 14.3~20.3
Parts by weight, most preferably 16.3~18.3 parts by weight.
The specifically chosen of the filler is not particularly limited the present invention, with anticorrosive paint well known to those skilled in the art
With filler, those skilled in the art can be selected according to practical situations, product requirement and quality requirement and
Adjustment, filler of the present invention preferably includes zinc powder, ferrophosphorus powder, aluminium powder, epoxy iron red shop, iron oxide red, mica sheet, glass squama
One or more in piece, calcium carbonate and talcum powder, more preferably zinc powder, ferrophosphorus powder, aluminium powder, epoxy iron red shop, iron oxide red, cloud
Two or more in master slice, glass flake, calcium carbonate and talcum powder.
The addition of the graphene and the composite of di-iron trioxide is not particularly limited the present invention, with this area
The proportioning of conventional di-iron trioxide in anticorrosive paint known to technical staff, those skilled in the art can answer according to actual
Selected and adjusted with situation, product requirement and quality requirement, graphene and di-iron trioxide of the present invention it is compound
The addition of material is preferably 35~65 parts by weight, more preferably 40~60 parts by weight, most preferably 45~55 parts by weight.
Selection of the present invention to the di-iron trioxide in the composite of the graphene and di-iron trioxide be not special
Limitation, with the selection of the conventional di-iron trioxide of anticorrosive paint well known to those skilled in the art, those skilled in the art
It can be selected and be adjusted according to practical situations, product requirement and quality requirement, di-iron trioxide of the present invention
Particle diameter be preferably 0.5 μm~5mm, more preferably 1 μm~1mm, most preferably more preferably 5~200 μm, 10~30 μm.
Definition of the present invention to the graphene in the composite of the graphene and di-iron trioxide is not particularly limited,
With the definition of graphene well known to those skilled in the art, those skilled in the art can be according to practical situations, production
Product requirement and quality requirement are selected and adjusted, and graphene of the present invention is preferably the graphene of broad sense, i.e. graphene
Class material, preferably includes the one or more in graphene, graphene oxide, redox graphene and modified graphene, more
Preferably graphene, graphene oxide, redox graphene or modified graphene, most preferably graphene.
The present invention is not limited especially the specifically compound mode in the composite of the graphene and di-iron trioxide
System, in compound mode well known to those skilled in the art, those skilled in the art can be according to practical situations, production
Product requirement and quality requirement are selected and adjusted, of the present invention compound to preferably include to spray, smear brush, doping, growth, sink
One or more in product, embedded, bonding, cladding and covering, more preferably spray, smear brush, doping, growth, deposition, insertion,
Bonding, cladding are covered, and are most preferably coated or are covered.The compound concrete form can also be compound for physics or chemical multiple
Conjunction form.Specifically, the composite of graphene of the present invention and di-iron trioxide is preferably the uniform composite graphite alkene in surface
Di-iron trioxide material.
The present invention is to graphene in the composite of the graphene and di-iron trioxide and the specific ratio of di-iron trioxide
Example is not particularly limited, with the ratio of graphene composite material well known to those skilled in the art, those skilled in the art
It can be selected and be adjusted according to practical situations, product requirement and quality requirement, graphene of the present invention and institute
The mass ratio of di-iron trioxide is stated, or the graphene accounts for the gross mass of the composite of the graphene and di-iron trioxide
Ratio can be preferably independently (0.01~1)：100, more preferably (0.05~0.8)：100, more preferably (0.1~0.6)：
100, be most preferably (0.2~0.5)：100.
The source of the graphene and the composite of di-iron trioxide is not particularly limited the present invention, with this area skill
Usual sources known to art personnel, commercially available purchase, can also voluntarily be prepared, and those skilled in the art can be according to reality
Border applicable cases, product requirement and quality requirement are selected and adjusted.
Above-mentioned steps of the present invention provide a kind of graphene/ferric oxide composite material, change graphite alkenes material
Addition manner, graphene and di-iron trioxide are combined first, the composite of graphene and di-iron trioxide is obtained, then
Again anticorrosive paint is combined into other compositions.Selection and proportion optimizing of the present invention by composition, in conjunction with a variety of auxiliary agents, are obtained
Using more extensive resin anti-corrosive paint.The resin anti-corrosive paint that the present invention is provided effectively solves ordinary graphite alkenes material
Material is difficult to ensure that dispersed, easily reunion and flexible inherent shortcoming；Although and being improved by the way of addition dispersant
The degree of scatter of graphene, but other impurities are readily incorporated, the drawbacks of can not also overcoming reunion；It it also avoid three in anticorrosive paint
The problem of aoxidizing high two iron contents and thick film layer.
Present invention also offers a kind of preparation method of resin anti-corrosive paint, comprise the following steps：
A graphene and di-iron trioxide) are obtained into the composite wood of graphene and di-iron trioxide after first mixing
Material；
B graphene and the composite of di-iron trioxide, resin and the solvent for) obtaining above-mentioned steps are mixed, warp
Cross after rotary evaporation again, obtain mixture；
C after the mixture and auxiliary agent for) obtaining above-mentioned steps are mixed again, resin anti-corrosive paint is obtained.
The present invention is to the selection of raw material and composition needed for above-mentioned preparation process, and corresponding optimum principle, and foregoing
The selection of corresponding raw material and composition in resin anti-corrosive paint, and corresponding optimum principle can carry out correspondence, herein not
Repeat one by one again.
The present invention after mixing, obtains the compound of graphene and di-iron trioxide first by graphene and di-iron trioxide
Material.
The design parameter of the graphene is not particularly limited the present invention, with well known to those skilled in the art conventional
The parameter of graphite alkenes material, those skilled in the art can want according to practical situations, product requirement and quality
Ask and selected and adjusted, in graphene of the present invention, the accounting that lamella is less than or equal to 5 layers of graphene is preferably greater than or equal to
80%, more preferably higher than equal to 85%, more preferably higher than equal to 90%.The piece footpath of graphene of the present invention is preferably 1
~100 μm, more preferably 10~90 μm, more preferably 30~70 μm, more preferably 40~60 μm, specifically most preferably 10~50
μm。
The present invention is to above-mentioned steps A), i.e., the specific preparation process of the composite of graphene and di-iron trioxide is without spy
Do not limit, with the blend step of graphene composite material well known to those skilled in the art, those skilled in the art can be with
Selected and adjusted according to practical condition, product requirement and quality requirement, the present invention aoxidizes to improve graphene/tri-
The performance of two iron composite materials, optimized process flow and the integrality for ensureing process route, the step A) it is particularly preferred as：
A1) by after graphene solution and ferric oxide particle uniformly mixing, mixture is obtained；
A2) mixture for obtaining above-mentioned steps obtains three oxygen of the dispersed graphene in surface after rotary evaporation
Change two iron particles.
The particle diameter of the di-iron trioxide is not particularly limited the present invention, with well known to those skilled in the art three oxidations
The particle diameter of two iron particles, those skilled in the art can enter according to practical condition, product requirement and quality requirement
Row selection and adjustment, the particle diameter of ferric oxide particle of the present invention is preferably 0.5 μm~5mm, more preferably 1 μm~1mm,
More preferably 5~200 μm, most preferably 10~30 μm.
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 process for dispersing of the graphene solution is not particularly limited the present invention, with well known to those skilled in the art point
Dissipate 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 ferric oxide particle is not particularly limited the present invention, with art technology
Conventional ratio known to personnel, those skilled in the art can want according to practical condition, product requirement and quality
Ask and selected and adjusted, the mass ratio of graphene of the present invention and the ferric oxide particle 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, tool
Body can be (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：
Ferric oxide particle is slowly added into the graphene solution after scattered, while uniform mixing, is obtained
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
Ferric oxide particle.
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 ferric oxide particle are combined closely,
The rotary speed of the rotary evaporation is preferably 40~70rpm, more preferably 45~65rpm, most preferably 50~60rpm.
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 ferric oxide particle are combined closely,
The temperature of the rotary evaporation is preferably 60~80 DEG C, more preferably 65~75 DEG C, most preferably 67~73 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 ferric oxide particle are combined closely,
The time of the rotary evaporation is preferably 0.5~2h, more preferably 0.7~1.8h, most preferably 0.5~1.5h, specifically can be with
For loosely powdered is finally presented with the ferric oxide particle for being compounded with 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 ferric oxide particle are combined closely,
The pressure of the rotary evaporation, which is preferably less than, is equal to 0.1MPa, more preferably under tiny structure or vacuum condition, most preferably exists
Under vacuum condition；Specific pressure is preferably 0.003~0.05MPa, more preferably 0.005~0.03MPa, more preferably 0.006
~0.01MPa, most preferably 0.007~0.009MPa.
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 further preferably employs rotation during the composite of graphene and di-iron trioxide is prepared
Evaporation technique, further preferably by controlling vacuum, rotary speed, revolving temperature (bath temperature) etc. to be coated in graphene uniform
Ferric oxide particle surface, untill material is in drying regime, so that by graphene, macroscopical or micron-sized di-iron trioxide
Particle is closely linked, and can effectively solve graphene dispersion problem of non-uniform, preferably plays its premium properties, and
And the ferric oxide particle material of grapheme material can also be obtain a uniformly coated, make graphene to the equal of ferric oxide particle
Even scatter coated becomes a reality.And the present invention is special under conditions of existing without protective gas, carries out aforesaid operations, from
And simplify production procedure, production equipment and reduce production consumption.Above-mentioned complex method technique that the present invention is provided is simple,
Mild condition, safety and environmental protection, are more suitable for the big production of technology.
The present invention is using the processing mode rotated, by the dispersed encapsulated of graphene uniform on ferric oxide particle surface,
The available graphene ferric oxide particle that can uniformly coat, i.e., dispersed graphene.Not only fundamentally solve
Graphene mixes uneven disadvantage in the solution, ensure that the dispersed of graphene, and graphene is coated on
Grain surface, it is ensured that its flat presentation of graphene reduces fold, its performance is preferably played, so as to solve stone well
Black alkene scattering problem, it is ensured that the perfect performance of its premium properties.
Composite, resin and the solvent of the graphene for then obtaining above-mentioned steps and di-iron trioxide of the invention are carried out
Mixing, after rotary evaporation again, obtains mixture.
The mode of the mixing is not particularly limited the present invention, with the mixing side of coating well known to those skilled in the art
Formula, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement,
Mixing of the present invention preferably includes stirring mixing and/or ultrasonic mixing, more preferably stirring mixing and ultrasonic mixing.
The specific steps and parameter of the mixing are not particularly limited the present invention, are applied with well known to those skilled in the art
The mixed process and parameter of material, those skilled in the art can want according to practical condition, product requirement and quality
Ask and selected and adjusted, the specific steps and parameter of mixing of the present invention are preferably completed with reference to relevant national standard,
The time of the mixing is preferably 1~2h, more preferably 1.2~1.8h, most preferably 1.4~1.6h, graphene in the present invention
Addition do not influence mixing the step of and parameter.
The present invention is to the step B) in the specific steps and parameter of rotary evaporation again be not particularly limited, with this area
The process and parameter of rotary evaporation known to technical staff, those skilled in the art can be according to practical condition, productions
Product requirement and quality requirement are selected and adjusted.
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 is improved preferably uniformly to mix the composite and other materials of graphene and di-iron trioxide with this
The dispersing uniformity of graphene, the rotary speed of the rotary evaporation again is preferably 40~70rpm, more preferably 45~
65rpm, most preferably 50~60rpm.
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 is improved preferably uniformly to mix the composite and other materials of graphene and di-iron trioxide with this
The dispersing uniformity of graphene, the temperature of the rotary evaporation again is preferably 60~80 DEG C, more preferably 65~75 DEG C, optimal
Elect 67~72 DEG C as.
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 is improved preferably uniformly to mix the composite and other materials of graphene and di-iron trioxide with this
The dispersing uniformity of graphene, the time of the rotary evaporation again is preferably 0.5~2h, and more preferably 0.8~1.8h is optimal
Elect 1~1.5h as.
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 is improved preferably uniformly to mix the composite and other materials of graphene and di-iron trioxide with this
The dispersing uniformity of graphene, the pressure of the rotary evaporation again, which is preferably less than, is equal to 0.1MPa, more preferably micro- negative
Under pressure or vacuum condition, most preferably under vacuum；Specific pressure is preferably 0.003~0.05MPa, and more preferably 0.005
~0.03MPa, more preferably 0.006~0.01MPa, most preferably 0.007~0.009MPa.
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.
After the last mixture for obtaining above-mentioned steps and auxiliary agent of the invention are mixed again, resin anti-corrosive paint is obtained.
The present invention is improves the application performance of resin anti-corrosive paint, and optimized process flow is complete with guarantee process route
Property, the step C) it is particularly preferred as：
C1 mixture, filler, anti-settling agent and the defoamer for) obtaining above-mentioned steps obtain resin after stirring mixing
The first component of anticorrosive paint；
By curing agent, accelerator and solvent after being again stirring for mixing, the second component of resin anti-corrosive paint is obtained；
C2 the first component and second component of above-mentioned steps) are obtained into resin anti-corrosive paint after mixing.
The species of the auxiliary agent is not particularly limited the present invention, is with Coatings Additives 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 situations, product requirement and quality requirement
The bright auxiliary agent preferably includes coating itself (first component) used additives and (second component) used additives, the first component when coating is used
Used additives preferably include the one or more in anti-settling agent, defoamer and filler, more preferably in anti-settling agent, defoamer and filler
It is a variety of；The second component used additives preferably include the one or more in curing agent, accelerator and solvent, more preferably solidify
It is a variety of in agent, accelerator and solvent.
The present invention to the step C1) in stirring mixing rotating speed be not particularly limited, it is ripe with those skilled in the art
The rotating speed of the stirring mixed process for the anticorrosive paint known, those skilled in the art can be according to practical condition, product
It is required that and quality requirement selected and adjusted, it is of the present invention stirring mixing be preferably high-speed stirred mixing, the rotating speed
Preferably 1000~2000rpm, more preferably 1200~1800rpm, more preferably 1300~1700rpm, most preferably 1400
~1600rpm.
The present invention to the step C1) in stirring mixing time be not particularly limited, it is ripe with those skilled in the art
The set of time of the stirring mixed process for the anticorrosive paint known, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and adjusted, and the time of stirring mixing of the present invention is preferably 1~3 hour, more
Preferably 1.2~2.7 hours, most preferably 1.5~2.5 hours.
The present invention to the step C1) in stirring mixing temperature be not particularly limited, it is ripe with those skilled in the art
The temperature setting of the stirring mixed process for the anticorrosive paint known, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and adjusted, and the temperature of stirring mixing of the present invention is preferably room temperature, specifically may be used
Think 10~40 DEG C, can be 15~35 DEG C, or 20~30 DEG C.
The present invention to the step C1) in be again stirring for mixing rotating speed be not particularly limited, with people in the art
Member known to anticorrosive paint stirring mixed process rotating speed, those skilled in the art can according to practical condition,
Product requirement and quality requirement are selected and adjusted, of the present invention to be again stirring for mixing preferably high-speed stirred mixing,
The rotating speed is preferably 1000~1500rpm, more preferably 1100~1400rpm, most preferably 1200~1300rpm.
The present invention to the step C1) in be again stirring for mixing time be not particularly limited, with people in the art
The set of time of the stirring mixed process of anticorrosive paint known to member, those skilled in the art can be according to actual production feelings
Condition, product requirement and quality requirement are selected and adjusted, and the time of the present invention for being again stirring for mixing is preferably 0.5~
2 hours, most preferably more preferably 0.8~1.8 hour, 1~1.5 hour.
The present invention to the step C1) in be again stirring for mixing temperature be not particularly limited, with people in the art
The temperature setting of the stirring mixed process of anticorrosive paint known to member, those skilled in the art can be according to actual production feelings
Condition, product requirement and quality requirement are selected and adjusted, the temperature preferably room temperature of the present invention for being again stirring for mixing,
It is specifically as follows 10~40 DEG C, can is 15~35 DEG C, or 20~30 DEG C.
The present invention changes traditional graphene addition manner, and graphene is wrapped in into three by chemistry or physics mode
Two iron particle surfaces are aoxidized, are then used further in post-coatings production.And new dispersing mode is further preferably employed, can
Fundamentally solve Flexible graphene and uneven disadvantage is mixed in coating system, ensure that the dispersed of graphene.
Graphene is wrapped in ferric oxide particle surface simultaneously, it is ensured that its flat presentation of graphene reduces fold, preferably
Play its performance.
The present invention is obtained after the first component and second component of above-mentioned resin anti-corrosive paint, can also carry out step C2)：
C2 the first component and second component for) obtaining above-mentioned steps obtain resin anti-corrosive paint after mixing.
The present invention to the step whether with C1) it is continuous that there is no particular restriction, those skilled in the art, which are based on general knowledge, to be known
Dawn, the step can be operated in anticorrosive paint using preceding, i.e., by C2) after step, resin anti-corrosive paint can enter enforcement
With.Therefore, in the preparation of resin anti-corrosive paint, can be free of has the step, can also equally not contain resin anti-corrosive paint
Second component.
The present invention to the step C2) in mixing specific steps and parameter be not particularly limited, with people in the art
Mixed process and parameter before coating use known to member, those skilled in the art can be according to practical situations, productions
Product requirement and quality requirement are selected and adjusted.
Above-mentioned steps of the present invention provide a kind of efficient, permanent salt spray resistance, the preparation side of the resin anti-corrosive paint of strong hardness
Method, changes the traditional approach that graphite alkenes material is directly appended in solution, graphite alkenes material is wrapped in into three oxygen first
Change two iron particle surfaces, then the ferric oxide particle after processing is added in anticorrosive paint, stone can be solved well
Black alkenes material scattering problem, it is ensured that the perfect performance of its premium properties；And other dispersants etc. need not be added other are miscellaneous
Random material, reduces the introducing of impurity, is effectively reduced negative effect of the pollutant to actual effect；Also greatly reduce three
The consumption of two iron is aoxidized, production cost is not only greatly lowered, the di-iron trioxide cigarette harm of human weld's process is also improved.
The present invention fundamentally solves soft graphite alkenes material and uneven disadvantage is mixed in coating system, ensure that graphite
Alkenes material it is dispersed, while graphite alkenes material is wrapped in into ferric oxide particle surface, it is ensured that graphene
With preferable its flat presentation, fold is reduced, its performance is preferably played.
Test result indicates that, the simple cost of preparation method technique that the present invention is provided is low, and the coating prepared has length
Long salt-fog resistant time, can reach 2110 hours, be 5 times of national standard, the paint film structure with high intensity and film thickness is thin,
The characteristics of shock resistance is strong, can reach 100g.cm, and environment-friendly.
In order to further illustrate the present invention, a kind of system of the resin anti-corrosive paint provided with reference to embodiments the present invention
Preparation Method is described in detail, but it is to be understood that these embodiments are carried out in fact lower premised on technical solution of the present invention
Apply, give detailed embodiment and specific operating process, simply to further illustrate the features and advantages of the present invention, and
It is not limiting to the claimed invention, protection scope of the present invention is also not necessarily limited to following embodiments.
Embodiment 1
Graphene/ferric oxide composite material
1) it is 0.5% graphene ethanol solution, ultrasonic agitation 3h to take content；
2) 250g di-iron trioxides are added slowly to step 1 under mechanical stirring according to the ratio of graphene 0.1%) in
In obtained graphene 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 50RPM is lasting to carry out, to material in dry
Untill dry state, the ferric oxide particle of the dispersed graphene in surface, i.e. graphene coating particles are obtained；
The graphene prepared to above-mentioned steps of the present invention/ferric oxide composite material carries out macroscopic analysis, three after coating
Aoxidize obvious color burn before two iron are relatively coated.
Electronic Speculum micro-analysis is scanned to graphene/ferric oxide composite material prepared by above-mentioned steps of the present invention,
Referring to Fig. 1, Fig. 1 is the SEM scannings of graphene/ferric oxide composite material microscopic appearance prepared by the embodiment of the present invention 1
Electromicroscopic photograph.Referring to Fig. 2, Fig. 2 is the SEM stereoscan photographs of common ferric oxide particle microscopic appearance.
From Fig. 1 and 2, graphene is uniformly attached to di-iron trioxide surface in the form of sheet, and the present invention is in three oxygen
Change two iron particle top layers and form graphene film layer, and the attachment of graphene film layer is uniform, has no agglomeration, thickness is 2nm
Left and right.
Resin anti-corrosive paint
1) take the above-mentioned contents of 50g to be modified di-iron trioxide, 40g epoxy resin for 0.1% graphene and be dissolved in 120g dimethylbenzene
With n-butanol with 3:The in the mixed solvent of 1 mixing, ultrasonic agitation 1h；
2) by step 1) gained mixed solution be added in rotary evaporator；
3) 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 viscous
Untill thick state；
4) by step 3) obtained by mixed material be added in high speed agitator, add 5.1g zinc oxide, 12.2g talcums
Powder, 2.8g organic pottery clays, 1g defoamers, 0.6g MONORAL 3300, high-speed stirred 30min, rotating speed 1500r/min；
5) by step 4) obtained mixture is added in three-roller and is ground to 25~55 μm, and first component is made.
Second component
6) it is 3 by weight by dimethylbenzene and n-butanol:1 is configured to mixed solvent 30g；
7) successively to step 6) in add stirring under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed until
It is uniformly dispersed, obtains second component.
8) anticorrosive paint in use, by the first and second components according to mass ratio 10:1 mixing.
Resin anti-corrosive paint prepared by the embodiment of the present invention 1 is detected.
Anticorrosive paint and the coating containing di-iron trioxide with formula prepared by above-mentioned steps, with electrolyte solution, polish,
Cleaning electrode；Then start instrument, preheat, open control software and assemble experimental provision again, after instrument state is normal, connection is led
Line；Selection measurement function, it is 0mV to 2000mV, sweep speed to set electric potential scanning scope：100mV/s, measurement polarization curve enters
The detection of row polarization curve carries out polarization curve detection.
Referring to Fig. 3, Fig. 3 is that resin anti-corrosive paint prepared by the embodiment of the present invention 1 and common anti-corrosion containing di-iron trioxide are applied
The polarization curve comparison diagram of material.
From the figure 3, it may be seen that the corrosion current Icorr=6.5e-006A/cm of the common di-iron trioxide coating with formula2；
And the corrosion current Icorr=10.5e-010A/cm for the di-iron trioxide coating that graphene is modified2, Comparatively speaking, corrosion electricity
Stream 4 orders of magnitude of reduction.
Performance detection is carried out to resin anti-corrosive paint prepared by the embodiment of the present invention 1.
Referring to table 1, the paint film property detection for the resin anti-corrosive paint that table 1 is prepared for the present invention.
Embodiment 2
1) take the above-mentioned contents of 50g to be modified di-iron trioxide, 50g epoxy resin for 0.1% graphene and be dissolved in 110g dimethylbenzene
With n-butanol with 3:The in the mixed solvent of 1 mixing, ultrasonic agitation 1h；
2) by step 1) gained mixed solution be added in rotary evaporator；
3) 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 viscous
Untill thick state；
4) by step 3) obtained by mixed material be added in high speed agitator, add 5.1g zinc oxide, 12.2g talcums
Powder, 2.8g organic pottery clays, 1g defoamers, 0.6g MONORAL 3300, high-speed stirred 30min, rotating speed 1500r/min；
5) by step 4) obtained mixture is added in three-roller and is ground to 25~55 μm, and first component is made.
Second component
6) it is 3 by weight by dimethylbenzene and n-butanol:1 is configured to mixed solvent 30g；
7) successively to step 6) in add stirring under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed until
It is uniformly dispersed, obtains second component.
8) anticorrosive paint in use, by the first and second components according to mass ratio 10:1 mixing.
Performance detection is carried out to resin anti-corrosive paint prepared by the embodiment of the present invention 2.
Referring to table 1, the paint film property detection for the resin anti-corrosive paint that table 1 is prepared for the present invention.
Embodiment 3
1) take the above-mentioned contents of 50g to be modified di-iron trioxide, 60g epoxy resin for 0.1% graphene and be dissolved in 100g dimethylbenzene
With n-butanol with 3:The in the mixed solvent of 1 mixing, ultrasonic agitation 1h；
2) by step 1) gained mixed solution be added in rotary evaporator；
3) 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 viscous
Untill thick state；
4) by step 3) obtained by mixed material be added in high speed agitator, add 5.1g zinc oxide, 12.2g talcums
Powder, 2.8g organic pottery clays, 1g defoamers, 0.6g MONORAL 3300, high-speed stirred 30min, rotating speed 1500r/min；
5) by step 4) obtained mixture is added in three-roller and is ground to 25~55 μm, and first component is made.
Second component
6) it is 3 by weight by dimethylbenzene and n-butanol:1 is configured to mixed solvent 30g；
7) successively to step 6) in add stirring under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed until
It is uniformly dispersed, obtains second component.
8) anticorrosive paint in use, by the first and second components according to mass ratio 5:1 mixing.
Performance detection is carried out to resin anti-corrosive paint prepared by the embodiment of the present invention 3.
Referring to table 1, the paint film property detection for the resin anti-corrosive paint that table 1 is prepared for the present invention.
Embodiment 4
1) take 50g contents to be modified di-iron trioxide, 70g epoxy resin for 0.3% graphene and be dissolved in 90g dimethylbenzene and positive fourth
Alcohol is with 3:The in the mixed solvent of 1 mixing, ultrasonic agitation 1h；
2) by step 1) gained mixed solution be added in rotary evaporator；
3) 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 viscous
Untill thick state；
4) by step 3) obtained by mixed material be added in high speed agitator, add 5.1g zinc oxide, 12.2g talcums
Powder, 2.8g organic pottery clays, 1g defoamers, 0.6g MONORAL 3300, high-speed stirred 30min, rotating speed 1500r/min；
5) by step 4) obtained mixture is added in three-roller and is ground to 25~55 μm, and first component is made.
Second component
6) it is 3 by weight by dimethylbenzene and n-butanol:1 is configured to mixed solvent 30g；
7) successively to step 6) in add stirring under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed until
It is uniformly dispersed, obtains second component.
8) anticorrosive paint in use, by the first and second components according to mass ratio 10:1 mixing.
Performance detection is carried out to resin anti-corrosive paint prepared by the embodiment of the present invention 4.
Referring to table 1, the paint film property detection for the resin anti-corrosive paint that table 1 is prepared for the present invention.
Embodiment 5
1) take the above-mentioned contents of 50g to be modified di-iron trioxide, 70g epoxy resin for 0.1% graphene and be dissolved in 100g dimethylbenzene
With n-butanol with 3:The in the mixed solvent of 1 mixing, ultrasonic agitation 1h；
2) by step 1) gained mixed solution be added in rotary evaporator；
3) 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 viscous
Untill thick state；
4) by step 3) obtained by mixed material be added in high speed agitator, add 5.1g zinc oxide, 12.2g talcums
Powder, 2.8g organic pottery clays, 1g defoamers, 0.6g MONORAL 3300, speed stirring 30min, rotating speed 1500r/min；
5) by step 4) obtained mixture is added in three-roller and is ground to 25~55 μm, and first component is made.
Second component
6) it is 3 by weight by dimethylbenzene and n-butanol:1 is configured to mixed solvent 30g；
7) successively to step 6) in add stirring under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed until
It is uniformly dispersed, obtains second component.
8) anticorrosive paint in use, by the first and second components according to mass ratio 10:1 mixing.
Performance detection is carried out to resin anti-corrosive paint prepared by the embodiment of the present invention 5.
Referring to table 1, the paint film property detection for the resin anti-corrosive paint that table 1 is prepared for the present invention.
Table 1
Above to a kind of resin anti-corrosive paint containing graphite alkenes/ferric oxide composite material for providing of the present invention and
Its preparation method is described in detail, and specific case used herein is carried out to the principle and embodiment of the present invention
Illustrate, the explanation of above example is only intended to the method and its core concept for helping to understand the present invention, including best mode, and
And also cause any person skilled in the art to put into practice the present invention, including any device or system are manufactured and use, and
Implement the method for any combination.It should be pointed out that for those skilled in the art, not departing from original of the invention
On the premise of reason, some improvement and modification can also be carried out to the present invention, these are improved and modification also falls into right of the present invention and wanted
In the protection domain asked.The scope of patent protection of the present invention is defined by the claims, and may include those skilled in the art
It is conceivable that other embodiment.If these other embodiments have the structure for being not different from claim character express will
Element, or if they include equivalent structural elements of the character express without essence difference with claim, then these other
Embodiment also should be comprising within the scope of the claims.
Claims (10)
1. a kind of resin anti-corrosive paint, it is characterised in that including resin, the composite of graphene and di-iron trioxide, auxiliary agent
And solvent.
2. resin anti-corrosive paint according to claim 1, it is characterised in that the resin is 25~55 parts by weight；
The composite of graphene and di-iron trioxide is 35~65 parts by weight；
Auxiliary agent is 17~32 parts by weight；
Solvent is 103~143 parts by weight；
The auxiliary agent includes the one or more in curing agent, accelerator, anti-settling agent, defoamer and filler.
3. resin anti-corrosive paint according to claim 2, it is characterised in that the curing agent is 1.5~3.5 parts by weight；
The accelerator is 0.05~0.2 parts by weight；
The anti-settling agent is 2.4~4.5 parts by weight；
The defoamer is 0.5~1.5 parts by weight；
The filler is 12.3~22.3 parts by weight.
4. resin anti-corrosive paint according to claim 3, it is characterised in that the graphene and di-iron trioxide it is compound
Material is the di-iron trioxide material of the uniform composite graphite alkene in surface；
The graphene includes the one or more in graphene oxide, graphene and modified graphene；
The resin includes one kind in epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin
Or it is a variety of；
The solvent include water, acetone, ethanol, isopropanol, butanone, 2-Pyrrolidone, dimethylbenzene, n-butanol, propene carbonate,
One or more in propylene glycol monomethyl ether and butyl acetate；
The defoamer includes organosiloxane defoamer, polyether antifoam agent and one kind or many in dimethicone defoamer
Kind；
The anti-settling agent includes anti-settling agent 3300, organic clay, organic pottery clay, aerosil, Tissuemat E and cellulose
One or more in ether；
The curing agent is included in polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, polyethylene polyamine and polyether diamine
One or more.
5. a kind of preparation method of resin anti-corrosive paint, it is characterised in that comprise the following steps：
A graphene and di-iron trioxide) are obtained into the composite of graphene and di-iron trioxide after first mixing；
B graphene and the composite of di-iron trioxide, resin and the solvent for) obtaining above-mentioned steps are mixed, by again
After secondary rotary evaporation, mixture is obtained；
C after the mixture and auxiliary agent for) obtaining above-mentioned steps are mixed again, resin anti-corrosive paint is obtained.
6. preparation method according to claim 5, it is characterised in that the step A) be specially：
A1) by after graphene solution and di-iron trioxide uniformly mixing, mixture is obtained；
A2) mixture for obtaining above-mentioned steps is after rotary evaporation, obtain the dispersed graphene in surface graphene and
Ferric oxide composite material.
7. preparation method according to claim 6, it is characterised in that the quality of the graphene and the di-iron trioxide
Than for (0.01~1): 100；
The step A1) in, the rotary speed of the rotary evaporation is 40~70rpm；
The temperature of the rotary evaporation is 60~80 DEG C；
The pressure of the rotary evaporation is 0.003~0.05MPa；
The time of the rotary evaporation is 0.5~2h.
8. preparation method according to claim 5, it is characterised in that the step B) in, the rotary evaporation again
Rotary speed is 40~70rpm；
The temperature of the rotary evaporation again is 60~80 DEG C；
The pressure of the rotary evaporation again is 0.003~0.05MPa；
The time of the rotary evaporation again is 0.5~2h.
9. the preparation method according to claim 5~8 any one, it is characterised in that the step C) be specially：
C1 mixture, filler, anti-settling agent and the defoamer for) obtaining above-mentioned steps obtain resin resistant after stirring mixing
The first component of coating；
By curing agent, accelerator and solvent after being again stirring for mixing, the second component of resin anti-corrosive paint is obtained；
The auxiliary agent includes the one or more in curing agent, accelerator, anti-settling agent, defoamer and filler.
10. preparation method according to claim 8, it is characterised in that the rotating speed of the stirring mixing for 1000~
2000rpm；The time of the stirring mixing is 1~3 hour；
The rotating speed for being again stirring for mixing is 1000~1500rpm；The time for being again stirring for mixing is 0.5~2 hour.
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