CN105647338B - With high insulating graphene/epoxy resin composite anticorrosion coating and preparation method - Google Patents

With high insulating graphene/epoxy resin composite anticorrosion coating and preparation method Download PDF

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Publication number
CN105647338B
CN105647338B CN201410712531.3A CN201410712531A CN105647338B CN 105647338 B CN105647338 B CN 105647338B CN 201410712531 A CN201410712531 A CN 201410712531A CN 105647338 B CN105647338 B CN 105647338B
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graphene
epoxy resin
component
coating
high insulating
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CN105647338A (en
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裴嵩峰
黄坤
任文才
成会明
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Deyang Peihua Carbon Material Technology Development Co.,Ltd.
Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The present invention relates to metal erosion to protect field, is specially a kind of graphene with high insulating/epoxy resin composite anticorrosion coating and preparation method.Graphene/epoxy resin masterbatch of the graphene content in 5wt% is added in ordinary epoxy resin, diluent is added and auxiliary agent stirring is allowed to be uniformly dispersed to form component A;B component is curing agent.By weight percentage, component A accounts for 53~93%, and B component accounts for 7~47%;In component A, the content range of graphene is 0.03~2.3wt%.Two components, which are mixed evenly, can prepare graphene/epoxy resin composite coating, and the corrosion protective coating with high insulating can be prepared after applying drying according to a conventional method.Compared with prior art, the graphene that the present invention prepares/epoxy coating graphene dosage is few, the advantages that can realizing that graphene is dispersed in composite coating at the same time, thus the splendid waterproof of coating, anticorrosive property, weatherability, resistance to acid and alkali, impact resistance and artificial ageing resistance can be assigned.

Description

With high insulating graphene/epoxy resin composite anticorrosion coating and preparation method
Technical field
The present invention relates to metal erosion to protect field, is specially that a kind of graphene/epoxy resin with high insulating is multiple Close anticorrosive paint and preparation method.
Background technology
Metal erosion is due to metal surface by chemistry or the electrochemical action of surrounding medium and destroyed phenomenon, anti-corrosion It is to coat erosion shield in metal surface to lose the most frequently used and effective method, and the corrosive medium such as matrix and water, oxygen is completely cut off.Cause This, the barrier property of coating makes one of principal element of evaluation anticorrosive paint performance.It is existing corrosion anticorrosive paint be typically with Polymer is main film forming substance, such as:Epoxy resin, alkyd resin, acrylic resin etc..Polymer is formed in film forming procedure Crystal defect, micro-crack, the inducing action of pinhole arrangement and polymer molecule segment polar groups, can all cause water, The infiltration of oxygen and corrosive ion in the coating, and appearing in film forming procedure for these structures is inevitable.Tradition Insulating corrosion protective coating in can be added into the fillers of some high insulating, such as:The sheets such as glass flake, mica sheet are filled out Material, different from plain particles shape filler, this kind of filler has big radius-thickness ratio (lamella lateral dimension/lamellar spacing), chemically Matter stablizes and corrosive medium the characteristics of being not through, their being uniformly distributed in the coating, can increase corrosion mechanism in the coating Diffusion path, make its be difficult to reach metal surface formed corrosion.
Graphene is a kind of novel nano Carbon Materials being made of carbon atom, its structure is that have carbon atom with sp2Hydridization rail Road composition honeycomb two dimensional crystal material, its thickness for one to several monoatomic layers (<3nm), lamella size is at a few micrometers To some tens of pm.Compared with traditional insulating filler, graphene has obviously advantage at following three aspects:
(1) face diameter/thickness ratio of bigger:The piece footpath of simple glass scale is usually tens of to hundreds of microns, and thickness is in number Hundred nanometers to a few micrometers of magnitude, its radius-thickness ratio is usually below 100;The piece footpath of graphene prepared by intercalation stripping method magnanimity leads to Often at a few micrometers to some tens of pm, and thickness is only 2~3 nanometers, its radius-thickness ratio is typically larger than 1000, and graphene is also not Permeable.Big radius-thickness ratio is more advantageous to suppressing the diffusion of corrosive medium in the coating;It means that the painting of same thickness Layer, graphene composite coating can realize the longer protection service life;On the other hand, graphene itself can also be utilized very thin and high The characteristics of effect barrier, prepare high performance thin layer corrosion protective coating or barrier coat.
(2) pliability:Compared with brittle glass flake or mica flake, graphene and its thin-film material be it is a kind of strong and Tough material, this property allow its composite coating preferably to resist damage caused by the effect of the external forces such as shock and vibration, friction Hinder and ensure excellent adhesive force, so as to improve the protection effect of coating.
(3) and the good combination power of polymer molecule:The C=C conjugated structures of graphene surface and the dangling bond knot at edge Structure allows it to form strong interaction between most polymers molecule, makes good between graphene sheet layer and resin material Good interface cohesion, so as to ensure good barriering effect and mechanical strength.
But since graphene has the characteristics that high-specific surface area and nanoscale, it is set to be carried out with fluoropolymer resin Easily to reunite during direct combination, i.e., graphene sheet layer flocks together, the little particle that formation does not disperse, rather than sheet Structure.This distributional pattern does not simply fail to improve the barrier property of coating, can form substantial amounts of hole knot in coat inside on the contrary Structure so that corrosive medium is easier to cause the corrosion of metallic matrix through coating.For this problem, applicants have invented " one The preparation method of kind nano-sized carbon/liquid resin masterbatch " (number of patent application:201410617460.9), it can be made based on this method It is standby go out weight percent concentration be 5wt% graphene/epoxy resin masterbatch, the graphene in this composite master batch is in height Dispersity, and can be diluted with the epoxy resin of identical type, and the scattered of graphene is kept in dilution State is constant, this method solves scattering problem of the graphene in coating application.
The content of the invention
It is an object of the invention to provide one kind to have high insulating graphene/epoxy resin composite anticorrosion coating and preparation Method, it is scattered to solve the problems, such as that graphene is difficult in insulating anticorrosive paint preparation process, prepares high-performance, low graphene High the insulating graphene/epoxy resin composite coating and coating of content.
The technical scheme is that:
One kind has high insulating graphene/epoxy resin composite anticorrosion coating, which is A, B two-component type, wherein: Component A includes epoxy resin, graphene/epoxy resin masterbatch, diluent, additive, and B component is curing agent;With epoxy resin Measure and be for 100 parts of weight meters, the weight composition of each component:
Component A:
B component:
20~100 parts of curing agent.
Described has high insulating graphene/epoxy resin composite anticorrosion coating, and by weight percentage, component A accounts for 53~93%, B component accounts for 7~47%.
Described has high insulating graphene/epoxy resin composite anticorrosion coating, in component A, the content of graphene Scope is 0.03~2.3wt%.
Described has high insulating graphene/epoxy resin composite anticorrosion coating, in component A, graphene/asphalt mixtures modified by epoxy resin Fat masterbatch is graphene and epoxy resin masterbatch compound resin slurry of the graphene content in 5 wt%.
Described has high insulating graphene/epoxy resin composite anticorrosion coating, and in component A, epoxy resin is double Phenol A type epoxy resin;Additive is the common auxiliary agent of paint field:Dispersant, defoamer, levelling agent and anti-settling agent one kind or Two or more mixing, dispersant, defoamer, levelling agent and the respective parts by weight of anti-settling agent are 0.5~2 part;Diluent is adopted Use organic solvent:One or both of toluene, dimethylbenzene, butanol, methyl ethyl ketone, cyclohexanone are mixed above.
Described has high insulating graphene/epoxy resin composite anticorrosion coating, and B component is amine, ethers or acid anhydrides Class curing agent.
The preparation method with high insulating graphene/epoxy resin composite anticorrosion coating, according to formula rate Epoxy resin, graphene/epoxy resin masterbatch, diluent and additive is added in blender at the uniform velocity to stir, rotating speed for 300~ 500 revs/min, stirring 1~3 it is small when, component A can be obtained by various materials is uniformly mixed packing;By two component of A, B in proportion After mixing, you can use.
The preparation method with high insulating graphene/epoxy resin composite anticorrosion coating, graphene/liquid tree The preparation method of fat masterbatch is:
Dry nano-sized carbon powder is added in alcoholic solvent stirring makes its complete wetting, using ultrasound, high-speed stirred or Shearing decentralized processing forms it into nano-sized carbon/alcohol suspension;It is molten to alcohol that nano-sized carbon/alcohol suspension is added into stirring in liquid resin Liquid and resin are layered, it is at the middle and upper levels milky to canescence low viscosity alcoholic solution, and lower floor is black high-viscosity material;By upper strata Alcoholic solution is with after lower floor's feed separation, collecting lower floor's material;The material of collection is carried out heating vacuumize it is dry after, that is, obtain The even compound resin slurry for being dispersed with nano-sized carbon, the upper strata alcoholic solution of collection after the Methods For Purification of distillation using reusing.
The preparation method with high insulating graphene/epoxy resin composite anticorrosion coating, 500g intercalations are shelled The graphene powder prepared from method is added in 30kg hexanols, and ultrasonic disperse 30 minutes, obtains graphene/alcohol that transient state is disperseed and hang Turbid;When mechanical agitation 5 is small after above-mentioned suspension is mixed with 10kg epoxy resin, mixing speed is 200 revs/min;Stirring After stand 10 minutes, be layered above-mentioned mixing liquid;The linen solution in upper strata is poured out, leaves the viscous of lower black Thick slurry material, inserts in vacuum drying oven to vacuumize and is heated to 120 DEG C, keeps vacuum in baking oven to be less than 100Pa;Dry 24 it is small when after Take out and obtain graphene/epoxy resin composite master batch of graphene content 5wt%.
The present invention design principle be:
There is the present invention high insulating graphene/epoxy resin composite anticorrosion coating to be made of two component of A, B, by weight hundred Point than for 5wt% graphene/epoxy resin masterbatch be added in ordinary epoxy resin add diluent and auxiliary agent stirring make Be uniformly dispersed to form component A, B component is epoxy curing agent.The graphene being dispersed in graphene/epoxy resin masterbatch Nanometer sheet homogeneously dispersed state in the form of sheets, is separated between graphene sheet layer by epoxy molecule, prevents graphene sheet layer Reunite;In dilution, the epoxy resin newly added can easily enter among graphene sheet layer, form low concentration Graphene epoxy composite coating retains dispersity of the graphene in coating at the same time, and this dispersity forms a film in paint solidification During will also be retained, and the laminal filter of high degree of dispersion is to form the basis of high insulating coating.
Beneficial effects of the present invention are as follows:
1st, only need simply to stir in dope preparing process of the present invention, you can realize the graphene high quality in coating point Dissipate so that the preparation process and technique of graphene composite coating simplify.
2nd, when graphene/epoxy coating for preparing of the present invention has an excellent barrier properties, it is necessary to graphene it is minimum Addition can be down to 0.2wt%.
3rd, graphene/epoxy coating prepared by the present invention, has good pliability and shock resistance.
4th, compared with prior art, graphene dosage is few, together for the graphene/epoxy coating prepared using the method for the present invention When can realize that graphene is dispersed in composite coating, thus the splendid waterproof of coating, anticorrosive property, weather-proof can be assigned The advantages that property, resistance to acid and alkali, impact resistance and artificial ageing resistance.
Brief description of the drawings
Fig. 1 epoxy coatings, epoxy resin/0.5wt% carbon blacks composite coating and epoxy resin/0.5wt% graphite Alkene composite coating water absorption rate with soaking time change curve.
Fig. 2 epoxy coatings, epoxy resin/0.5wt% carbon blacks composite coating and epoxy resin/0.5wt% graphite Alkene composite coating ion transmission with soaking time change curve.
Fig. 3 have good flexible graphene/epoxy resin composite coating and brittle epoxy coating picture. Wherein, (a) figure is 0.5wt% graphenes/epoxy resin laminated film (flexibility);(b) figure is epoxy resin thin film (brittleness).
Graphene/epoxy resin composite coating of Fig. 4 difference graphene additive amounts and commercial epoxy zinc-rich coating and ring Coating morphology after oxygen glass flake coatings soak 30 days in acid, alkali and neutral corrosive environment contrasts.Wherein, it is acid rotten Erosion uses 10wt% hydrochloric acid, and alkaline corrosion uses 10wt%NaOH aqueous solutions, and neutral salt corrosion uses 10wt%NaCl aqueous solutions, 1# represents graphene/epoxy composite coating of the graphene content as 0.5wt%, and 2# represents graphite of the graphene content as 1wt% Alkene/epoxy composite coating, 3# represent graphene/epoxy composite coating of the graphene content as 1.5wt%, and 4# represents typical commercial Epoxy zinc-rich coating, 5# represent typical commercial epoxy glass flake coating.
Embodiment
In a specific embodiment, the present invention has high insulating graphene/epoxy resin composite anticorrosion coating for A, B pairs Component-type, wherein:Component A includes material, the B components such as epoxy resin, graphene/epoxy resin masterbatch, diluent, additive Curing agent.The weight of each component forms (being counted by 100 parts of weight of amount of epoxy):
Component A:
B component:
20~100 parts of curing agent;
In component A, epoxy resin is mainly bisphenol A type epoxy resin, its trade mark is such as:E-20(601)、E-44 (6101), E-51 (618) etc..Additive is the common auxiliary agent of paint field, using commercial dispersants, defoamer, levelling agent and The mixing of the one or more of anti-settling agent.Preferably, dispersant, defoamer, levelling agent and the respective parts by weight of anti-settling agent Number is 0.5~2 part.Diluent uses organic solvent:One or both of toluene, dimethylbenzene, butanol, methyl ethyl ketone, cyclohexanone It is mixed above.
In component A, 5 wt% graphenes/epoxy resin masterbatch refers to Chinese invention patent application:A kind of " nanometer The preparation method (application number 201410617460.9) of carbon/liquid resin masterbatch ".Graphene/liquid resin masterbatch refers to stone For black alkene content in the compound resin slurry of 5wt%, graphene is dispersed wherein, and can be diluted into the compound of low concentration Resin, and dilute after graphene dispersity it is constant, the masterbatch application when dispersion performance it is good.Grapheme material can be low Realize the scattered of transient state in level alcoholic solvent, while lower alcohol solvent is also liquid resinous poor solvent, resin wherein molten Xie Du is very low.But resin dissolving micro in alcohol allows itself and graphene to form good combination, make graphene and tree Interaction force between fat gradually strengthens.Graphene is macroscopically shown as gradually to be transferred in resin from alcoholic solution, and shape Into dispersed.After being transferred to during graphene is completely by alcohol in resin, alcoholic solution will be layered with resin under static conditions. Since the combination power between alcoholic solution and resin is very weak, by the processing method of thermal evaporation it can be made to be kept completely separate with resin.
B component is amine, ethers or acid anhydride type curing agent, including:Polyamide, commercially available D8 (keto-aldehyde epoxide and fat The polynary amine additives of fat race), T31 (phenol aldehyde modified amine additives), 701# (phenol formaldehyde (PF) hexamethylene diamine condensation product), 704# (2- first Base imidazoles-epoxy propane butyl ether addition product), 705# (2-methylimidazole-glycidyl iso-octyl ether addition product), 70# acid anhydrides (butadiene-maleic anhydride addition compound), 308 tung oil acid anhydrides (tung oil-modified maleic anhydride) etc. it is one or two kinds of with On mixing.
The preparation process of anticorrosive paint of the present invention is as follows:
Epoxy resin, graphene/epoxy resin masterbatch, diluent and additive are added in blender according to formula rate When at the uniform velocity stirring (rotating speed is 300~500 revs/min) 1~3 is small, component A can be obtained by various materials is uniformly mixed packing. After two component of A, B is mixed in proportion, you can use.By weight percentage, component A accounts for 53~93%, and B component accounts for 7 ~47%;In component A, the content range of graphene is 0.03~2.3wt%, and preferred scope is 0.2~1.5wt%.Routinely After method applies drying, you can prepare the corrosion protective coating with high insulating.
In the following, by embodiment, the present invention is described in more detail.
Embodiment 1
Graphene powder prepared by 500g intercalations stripping method is added in 30kg hexanols, ultrasonic disperse 30 minutes, can obtain The graphene disperseed to transient state/alcohol suspension;When mechanical agitation 5 is small after above-mentioned suspension is mixed with 10kg epoxy resin, stir Speed is mixed as 200 revs/min;10 minutes are stood after stirring, is layered above-mentioned mixing liquid;By the linen solution in upper strata Pour out, leave the viscous paste of lower black, insert in vacuum drying oven to vacuumize and be heated to 120 DEG C, keep vacuum in baking oven Less than 100 Pa;Dry 24 it is small when after take out and obtain graphene/epoxy resin composite master batch of graphene content about 5wt%.
Count in parts by weight, the raw material composition of composite anticorrosion coating is as follows:
The component of component A is:
100 parts of epoxy resin;
5wt% graphenes/15 parts of epoxy resin masterbatch;
Solvent includes following component and ratio:
15 parts of dimethylbenzene;
15 parts of cyclohexanone;
15 parts of n-butanol;
Additive includes following component and ratio:
The component of component B is:
5 parts of kymene.
In the present embodiment, the preparation process of anticorrosive paint is as follows:
(1) the component A raw materials of above-mentioned weight ratio are uniformly mixed;
(2) can be used after mixture obtained by step (1) is uniformly mixed with polyamide by weight compatibility.
(3) content of graphene is about 0.5wt% in above-mentioned coating, and mixed coating is made independence using spread coating Film carry out it is resistance to infiltration and Mechanics Performance Testing and brush be made in carbon steel test piece coating test corrosion protection.
As shown in Figure 1, test result shows, the water absorption rate after graphene composite coating soaks 50 days is epoxy coating 1/10, be the 1/5 of identical addition carbon black composite coating.This is because the hydrophobicity of graphene in itself, and graphene Big lamellar structure can effectively suppress infiltration of the hydrone in coating, so as to significantly improve the anti-of epoxy resin-matrix coating Rotten performance.
As shown in Fig. 2, the addition of graphene can be with the suppression ion of highly significant in epoxy coating transmitance. Corrosive ion (such as Cl-) contacting metal surface is an important factor for causing metal erosion to aggravate, suppress the saturating of corrosive ion Cross be coating corrosion protection a key index.In graphene composite coating, Cl-The transmission rates of ion can be down to pure ring About the 1/100 of oxygen coating.
As shown in Fig. 3 (a)-(b), the addition of graphene can effectively improve the toughness and impact resistance of dope layer, protect The integrality of coating is demonstrate,proved, also just extends the service life of corrosion-inhibiting coating.
The above results show that the addition of graphene can effectively improve the isolation performance of coating, prepare with high isolation Graphene/epoxy resin composite coating of property.
Embodiment 2
Count in parts by weight, the raw material composition of composite anticorrosion coating is as follows:
The component of component A is:
100 parts of epoxy resin;
5wt% graphenes/6 parts of epoxy resin masterbatch;
Solvent includes following component and ratio:
15 parts of dimethylbenzene;
15 parts of cyclohexanone;
15 parts of n-butanol;
Additive includes following component and ratio:
The component of component B is:
25 parts of polyamide.
The content of graphene is about 0.2wt% in above-mentioned coating.It is made using preparation process same as Example 1 compound Film and coating, and identical performance test is carried out, it can obtain and 1 approximate test result of embodiment.Illustrate that graphene exists Graphene/epoxy resin composite coating of high insulating can be prepared in the case of extremely low addition.
Embodiment 3
Count in parts by weight, the raw material composition of composite anticorrosion coating is as follows:
The component of component A is:
100 parts of epoxy resin;
5wt% graphenes/50 parts of epoxy resin masterbatch;
Solvent includes following component and ratio:
20 parts of dimethylbenzene;
30 parts of n-butanol;
Additive includes following component and ratio:
The component of component B is:
100 parts of polyamide.
The content of graphene is about 1wt% in above-mentioned coating.THIN COMPOSITE is made using preparation process same as Example 1 Film and coating, and identical performance test is carried out, it can obtain and 1 approximate test result of embodiment.
Embodiment 4
Count in parts by weight, the raw material composition of composite anticorrosion coating is as follows:
The component of component A is:
100 parts of epoxy resin;
5wt% graphenes/60 parts of epoxy resin masterbatch;
Solvent includes following component and ratio:
15 parts of dimethylbenzene;
15 parts of cyclohexanone;
15 parts of n-butanol;
Additive includes following component and ratio:
The component of component B is:
40 parts of polyamide.
The content of graphene is about 1.5wt% in above-mentioned coating.It is made using preparation process same as Example 1 compound Film and coating, and identical performance test is carried out, it can obtain and 1 approximate test result of embodiment.
By the coating prepared by embodiment 1,3 and 4 and Commercial epoxy zinc-rich coating and epoxy glass flake coating in acid Property, carry out immersion corrosion test in 30 days in alkalescence and neutral salt corrosive liquid, acquired results are as shown in Figure 4.The result shows that either In acid, alkali or strong brine, graphene anticorrosive paint all maintains good protection effect, and being tested when 720 is small does not have finally There is phenomena such as corrosion, bubbling, rupture, and there is different degrees of corrosion in glass flake and zinc powder anticorrosive paint, illustrate stone Black alkene/epoxy resin composite coating can be used as a kind of high performance metal erosion protective coating.

Claims (7)

1. one kind has high insulating graphene/epoxy resin composite anticorrosion coating, it is characterised in that the coating is the double groups of A, B Part type, wherein:Component A includes epoxy resin, graphene/epoxy resin masterbatch, diluent, additive, and B component is curing agent; Counted by 100 parts of weight of amount of epoxy, the weight composition of each component is:
Component A:
100 parts of epoxy resin;
Graphene/1~100 part of epoxy resin masterbatch;
10~50 parts of diluent;
1~5 part of additive;
B component:
20~100 parts of curing agent;
In component A, graphene/epoxy resin masterbatch is that graphene and epoxy resin masterbatch of the graphene content in 5 wt% are answered Resin slurry, is dispersed in graphene nanometer sheet in graphene/epoxy resin masterbatch homogeneously dispersed state in the form of sheets, graphene Separated between lamella by epoxy molecule, prevent the reunion of graphene sheet layer;
The preparation method of graphene/liquid resin masterbatch is:
Dry nano-sized carbon powder is added to stirring in alcoholic solvent makes its complete wetting, utilizes ultrasound, high-speed stirred or shearing Decentralized processing forms it into nano-sized carbon/alcohol suspension;Will nano-sized carbon/alcohol suspension add in liquid resin stirring to alcoholic solution with Resin be layered, its at the middle and upper levels for milky to canescence low viscosity alcoholic solution, lower floor is black high-viscosity material;Upper strata alcohol is molten Liquid is with after lower floor's feed separation, collecting lower floor's material;The material of collection is carried out heating vacuumize it is dry after, i.e., uniformly divided Dissipating has the compound resin slurry of nano-sized carbon, and the upper strata alcoholic solution of collection after the Methods For Purification of distillation using reusing.
2. described in accordance with the claim 1 have high insulating graphene/epoxy resin composite anticorrosion coating, it is characterised in that By weight percentage, component A accounts for 53~93%, and B component accounts for 7~47%.
3. described in accordance with the claim 1 have high insulating graphene/epoxy resin composite anticorrosion coating, it is characterised in that In component A, the content range of graphene is 0.03~2.3wt%.
4. described in accordance with the claim 1 have high insulating graphene/epoxy resin composite anticorrosion coating, it is characterised in that In component A, epoxy resin is bisphenol A type epoxy resin;Additive is the common auxiliary agent of paint field:Dispersant, defoamer, The mixing of the one or more of levelling agent and anti-settling agent, dispersant, defoamer, levelling agent and the respective parts by weight of anti-settling agent Number is 0.5~2 part;Diluent uses organic solvent:One or both of toluene, dimethylbenzene, butanol, methyl ethyl ketone, cyclohexanone It is mixed above.
5. described in accordance with the claim 1 have high insulating graphene/epoxy resin composite anticorrosion coating, it is characterised in that B Component is amine, ethers or acid anhydride type curing agent.
6. the preparation method with high insulating graphene/epoxy resin composite anticorrosion coating described in a kind of claim 1, its It is characterized in that, adds epoxy resin, graphene/epoxy resin masterbatch, diluent and addition in blender according to formula rate Agent is at the uniform velocity stirred, and when rotating speed is 300~500 revs/min, stirring 1~3 is small, A can be obtained by various materials is uniformly mixed packing Component;After two component of A, B is mixed in proportion, you can use.
7. according to the preparation method with high insulating graphene/epoxy resin composite anticorrosion coating described in claim 6, its It is characterized in that, graphene powder prepared by 500g intercalations stripping method is added in 30kg hexanols, ultrasonic disperse 30 minutes, obtains The graphene that transient state is disperseed/alcohol suspension;When mechanical agitation 5 is small after above-mentioned suspension is mixed with 10kg epoxy resin, stirring Speed is 200 revs/min;10 minutes are stood after stirring, is layered above-mentioned mixing liquid;The linen solution in upper strata is fallen Go out, leave the viscous paste of lower black, insert in vacuum drying oven to vacuumize and be heated to 120 DEG C, keep vacuum in baking oven low In 100 Pa;Dry 24 it is small when after take out and obtain graphene/epoxy resin composite master batch of graphene content 5wt%.
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CN104087125B (en) * 2014-07-28 2017-04-05 南京航空航天大学 A kind of ocean Epoxy zinc-rich anticorrosive powdery paint and preparation method thereof
CN104177895A (en) * 2014-07-30 2014-12-03 重庆领先新材料有限公司 Graphene or graphite oxide-based anticorrosive coating and preparation method thereof
CN104140639B (en) * 2014-08-01 2016-08-24 黑龙江大学 A kind of preparation method of Graphene/epoxy resin composite material
CN104194455A (en) * 2014-08-25 2014-12-10 鸿纳(东莞)新材料科技有限公司 Graphene coating as well as preparation method and coating method thereof
CN104449249A (en) * 2014-11-04 2015-03-25 南京航空航天大学 Epoxy resin coating in marine steel pipe 3PE anticorrosive coating and preparation method thereof
CN104449208A (en) * 2014-11-05 2015-03-25 南京航空航天大学 3PE anticorrosive paint epoxy bottom layer for outer wall of deep sea oil and gas transmission steel pipe and preparation method of 3PE anticorrosive paint epoxy bottom layer

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