CN107099217A - A kind of resin anti-corrosive paint containing graphene/zinc powder composite and preparation method thereof - Google Patents

A kind of resin anti-corrosive paint containing graphene/zinc powder composite and preparation method thereof Download PDF

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Publication number
CN107099217A
CN107099217A CN201710292674.7A CN201710292674A CN107099217A CN 107099217 A CN107099217 A CN 107099217A CN 201710292674 A CN201710292674 A CN 201710292674A CN 107099217 A CN107099217 A CN 107099217A
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China
Prior art keywords
graphene
resin
zinc powder
present
composite
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CN201710292674.7A
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Inventor
刘海波
张在忠
李伟铭
赵永彬
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Shandong Oubo New Material Co Ltd
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Shandong Oubo New Material Co Ltd
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Priority to CN201710292674.7A priority Critical patent/CN107099217A/en
Publication of CN107099217A publication Critical patent/CN107099217A/en
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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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/103—Anti-corrosive paints containing metal dust containing Al
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C09D5/10—Anti-corrosive paints containing metal dust
    • C09D5/106—Anti-corrosive paints containing metal dust containing Zn
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0812—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0893—Zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention provides a kind of resin anti-corrosive paint, including, the composite and solvent of resin, graphene and zinc powder.The present invention changes the addition manner of graphite alkenes material, zinc powder in graphene and coating is combined first, obtain the composite of graphene and zinc powder, then the graphene and the composite particles of zinc powder 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 zinc powder, it can ensure that its flat presentation of graphene reduces fold, preferably play its performance.

Description

A kind of resin anti-corrosive paint containing graphene/zinc powder composite and its preparation Method
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/zinc powder composite 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 The two dimensional crystal of only one layer of atomic thickness of carbon atom composition, it is the current material most thin in application field and most of entering Tough material, 200 times more taller than steel of fracture strength also has elasticity well, and stretch range can reach own dimensions 20%；Meanwhile, graphene also has excellent electric conductivity, can reduce internal resistance, improves the cyclical stability of ultracapacitor； In addition, graphene is almost fully transparent, 2.3% light is only absorbed, and it is very fine and close, even minimum gas is former Sub (helium atom) can not also be penetrated.These features cause it to be highly suitable for a variety of subjects and field, also just because of graphite Alkene has above-mentioned many excellent physical chemical property, and it extensively should at energy storage material, environmental project, sensing sensitive aspect With, it is referred to as " dark fund " or " king of new material ", and potential application prospect is vast, has turned into global close at present Focus and study hotspot are noted, while also having moved towards industrialization from conceptual phase on derivatives such as graphenes, each row is caused each The wide participation of industry.
At present, the derivative such as graphene or graphene oxide, i.e. graphite alkenes material, can be used as preferably addition Material, imparts the new feature of composite, has expanded the application field of graphene composite material.Such as graphene or oxygen Graphite 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 The performance of product.And from world wide, all material because of the weight of corrosion loss about 1%, corrodes what is brought every year Economic 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 The loss that only marine corrosion is brought is with regard to the 3% of super GDP, and anti-corrosion road is shouldered heavy responsibilities.Make a general survey of domestic ocean engineering, shipbuilding And the industry fast development such as green marine wind energy, industrial antisepsis coating and field of coating enter the gold period of fast growth, Its market scale has been only second to building coating in various coating varieties and has occupied second.In recent years, China set on basis Apply construction, cities and towns My Perspective On The Co-building and new countryside construction, the Olympic Games, the Asian Games, the maximum Disney of Shanghai World's Fair and the whole world Shanghai etc. is settled in paradise, suffers from huge coating demand, is coating industry under new international situation and national policy And the fast development of industrial antisepsis coating provides new opportunity, greatly develops new anti-corrosion coating, has broad prospects and show Sincere justice.
In recent years, the coating products containing graphite alkenes material gradually have relevant report, but in actual applications, The problem of graphene also has many and restraining factors, such as graphene are easily reunited.Because graphene and its derivative compare table Area is larger, there is stronger model ylid bloom action power each other, reunites and wrapping phenomena is obvious, prevent it from stable dispersion, point Also easily reunite again after dissipating and be difficult to open together.Although have numerous studies by add different types of dispersant or Modified mode improves the dispersion effect of graphene, but effect is poor in practical application, and also to additionally introduce other miscellaneous Matter, is adversely affected to follow-up study, and when being mixed with hard material, is also easy to occur curling fold, these are all The effect that graphite alkenes material can be played will be directly affected.
Therefore, a kind of graphene/zinc powder composite how is obtained so that graphene can be in coating system more preferably Distribution, be to influence the key factor of coating property, be also many application vendors and a line research staff is urgently to be resolved hurrily asks Topic.
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/zinc powder composite and its system Preparation Method, graphene/zinc powder composite that the present invention is provided, graphene can be dispersed, and graphene has in composite There are preferable its flat presentation, less fold, so that with better performance.
The invention provides a kind of resin anti-corrosive paint, including, the composite and solvent of resin, graphene and zinc powder.
It is preferred that, the resin is 230~330 parts by weight；
The composite of graphene and zinc powder is 220~280 parts by weight；
Solvent is 176~236 parts by weight；
The resin anti-corrosive paint also includes auxiliary agent.
It is preferred that, the auxiliary agent includes one kind in curing agent, accelerator, dispersant, anti-settling agent, defoamer and filler Or it is a variety of；
The curing agent is 2~8 parts by weight；
The dispersant is 1~2 parts by weight；
The accelerator is 0.1~0.4 parts by weight；
The anti-settling agent is 2~3 parts by weight；
The defoamer is 2~4 parts by weight；
The filler is 20~40 parts by weight.
It is preferred that, the composite of the graphene and zinc powder is the zinc powder 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 is included in epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin 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 dispersant includes propene carbonate, Tissuemat E, polyacrylic acid sodium salt, styrene-maleic acid half ester Thing, styrene acrylic copolymer, acrylic acrylate copolymer, polyvinylpyrrolidone, polyurethane, polyethylene glycol and One or more in polyvinyl alcohol；
The defoamer includes one kind in organosiloxane defoamer, polyether antifoam agent and 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.
The invention provides a kind of preparation method of resin anti-corrosive paint, comprise the following steps：
A graphene and zinc powder) are obtained into the composite of graphene and zinc powder after first mixing；
B graphene and the composite of zinc powder, resin and the solvent for) obtaining above-mentioned steps are mixed, by again After rotary evaporation, resin anti-corrosive paint is obtained.
It is preferred that, the step A) be specially：
A1) by after graphene solution and zinc powder 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 zinc powder composite.
It is preferred that, the mass ratio of the graphene and the zinc powder is (0.01~1)：100；
The step A2) 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 0.5~1.5h.
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；
The step B) also include step C afterwards)；
C after) material and auxiliary agent after rotary evaporation again are mixed again, resin anti-corrosive paint is obtained.
It is preferred that, the step C) be specially：
C1) material after rotary evaporation again, filler, dispersant, anti-settling agent and defoamer are mixed by stirring Afterwards, the first component of resin anti-corrosive paint is obtained；
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, dispersant, anti-settling agent, defoamer and filler.
It is preferred that, the rotating speed of the stirring mixing is 1000~3000rpm；The time of the stirring mixing is 1~3h；
The rotating speed for being again stirring for mixing is 1000~3000rpm；The time for being again stirring for mixing for 0.5~ 2h。
The invention provides a kind of resin anti-corrosive paint, including, the composite and solvent of resin, graphene and zinc powder. Compared with prior art, the problem of present invention easily reunites for graphene, and the different degrees of presence of existing process for dispersing Reunite again, disperse inequality, introduce impurity, influence performance and the defect for improving processing cost.And be applied to apply During material, it is found that directly mixing or addition dispersant are unable to solve graphene agglomeration traits, it is difficult to ensure uniform point Dissipate, it is and flexible, it is also easy to introduce impurity, and then cause that anticorrosive paint salt-fog resistant time is short, shock resistance is poor and film The many defects of thickness etc..The addition manner for changing graphite alkenes material of the invention, first by graphene and Hard material in coating -- zinc powder is combined, and obtains the composite of graphene and zinc powder, then by the graphite after processing The composite particles of alkene and zinc powder are combined with other compositions, obtain resin anti-corrosive paint, graphene dispersion can be solved well and asked Topic, it is ensured that the perfect performance of its premium properties, and other auxiliary agents need not be added, the introducing of impurity is reduced, fundamentally Solve soft graphite alkenes material and uneven disadvantage mixed in coating system, ensure that the dispersed of graphene, While the composite of graphene and zinc powder, it is ensured that its flat presentation of graphene reduces fold, preferably plays its property Energy.
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 that the TEM transmission electron microscopes of graphene/zinc composite microscopic appearance prepared by the embodiment of the present invention 1 shine Piece；
Fig. 2 is the TEM transmission electron microscope photos of common zinc particle microscopic appearance；
Fig. 3 is the polarization curve contrast of resin anti-corrosive paint prepared by the embodiment of the present invention 1 and common zinc-rich anti-corrosive paint Figure；
Fig. 4 is the cross-section structure of anticorrosive paint SEM ESEMs prepared by the embodiment of the present invention 2；
Fig. 5 is the cross-section structure of the SEM ESEMs of common zinc-rich anti-corrosive paint.
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, the composite and solvent of resin, graphene and zinc powder.
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 according to practical situations, product requirement and quality requirement, this The resin is invented to preferably include in epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin One or more, more preferably epoxy resin, acrylic resin, polyaniline resin, fluorocarbon resin or superchlorinated polyvinyl chloride resin, Most preferably epoxy resin, acrylic resin or fluorocarbon resin.
The other specification of the resin is not particularly limited the present invention, with conventional tree well known to those skilled in the art The parameter of fat, 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, with resin resistant well known to those skilled in the art The proportioning of the usual resins of coating, those skilled in the art can be according to practical situations, product requirement and quality It is required that selected and adjusted, the addition of resin of the present invention is preferably 230~330 parts by weight, more preferably 250~ 310 parts by weight, most preferably 270~290 parts by weight.
The specifically chosen of the solvent is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art Material 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 includes water, acetone, ethanol, isopropanol, butanone, 2-Pyrrolidone, dimethylbenzene, positive fourth One or more in alcohol, propene carbonate, propylene glycol monomethyl ether and butyl acetate, more preferably water, acetone, ethanol, isopropyl Alcohol, butanone, 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, with resin resistant well known to those skilled in the art The proportioning of the Conventional solvents of coating, those skilled in the art can be according to practical situations, product requirement and quality It is required that selected and adjusted, the addition of solvent of the present invention is preferably 176~236 parts by weight, more preferably 186~ 226 parts by weight, most preferably 196~216 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.
The species of the auxiliary agent is not particularly limited the present invention, is helped with anticorrosive paint well known to those skilled in the art Agent, those skilled in the art can be selected and be adjusted according to practical situations, product requirement and quality requirement It is whole, auxiliary agent of the present invention preferably include one kind in curing agent, accelerator, dispersant, anti-settling agent, defoamer and filler or It is a variety of, preferably in curing agent, accelerator, dispersant, anti-settling agent, defoamer and filler two or more, or Gu Agent, accelerator, dispersant, anti-settling agent, defoamer or filler.
The addition of the curing agent is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art Conventional solidified dose of proportioning of material, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being adjusted, the addition of curing agent of the present invention is preferably 2~8 parts by weight, more preferably 3~7 weight Part, most preferably 4~6 parts by weight.
The specifically chosen of the curing agent is not particularly limited the present invention, with anti-corrosion well known to those skilled in the art Coating curing agent, those skilled in the art can be carried out according to practical situations, product requirement and quality requirement Selection and adjustment, curing agent of the present invention preferably include polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, many second One or more in alkene polyamines and polyether diamine, more preferably polyamide, ethylenediamine, diethylenetriamine, triethylene tetramine, Polyethylene polyamine or polyether diamine, are particularly preferred as polyamide 200.
The addition of the accelerator is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art The proportioning of the conventional accelerator of material, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being adjusted, the addition of accelerator of the present invention is preferably 0.1~0.4 parts by weight, more preferably 0.15 ~0.35 parts by weight, most preferably 0.2~0.3 parts by weight.
The specifically chosen of the accelerator is not particularly limited the present invention, with anti-corrosion well known to those skilled in the art Coating can be carried out with accelerator, those skilled in the art according to practical situations, product requirement and quality requirement Selection and adjustment, accelerator of the present invention preferably include DMP-30.
The addition of the dispersant is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art The proportioning of the conventional dispersant of material, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being adjusted, the addition of dispersant of the present invention is preferably 1~2 parts by weight, more preferably 1.2~1.8 Parts by weight, most preferably 1.4~1.6 parts by weight.
The specifically chosen of the dispersant is not particularly limited the present invention, with anti-corrosion well known to those skilled in the art Coating dispersant, those skilled in the art can be carried out according to practical situations, product requirement and quality requirement Selection and adjustment, the preferred propene carbonate of dispersant of the present invention, Tissuemat E, polyacrylic acid sodium salt, styrene-Malaysia It is sour half ester compound, styrene acrylic copolymer, acrylic acrylate copolymer, polyvinylpyrrolidone, polyurethane, poly- One or more in ethylene glycol and polyvinyl alcohol, more preferably propene carbonate, Tissuemat E, polyacrylic acid sodium salt, benzene second It is alkene-acid half ester compound, styrene acrylic copolymer, acrylic acrylate copolymer, polyvinylpyrrolidone, poly- Urethane, polyethylene glycol or polyvinyl alcohol, most preferably propene carbonate.
The addition 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 The proportioning of the conventional anti-settling agent of material, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being adjusted, the addition of anti-settling agent of the present invention is preferably 2~3 parts by weight, more preferably 2.2~2.8 Parts by weight, most preferably 2.4~2.6 parts by weight.
The specifically chosen of the anti-settling agent is not particularly limited the present invention, with anti-corrosion well known to those skilled in the art Coating anti-settling agent, those skilled in the art can be carried out according to practical situations, product requirement and quality requirement Selection and adjustment, anti-settling agent of the present invention preferably include anti-settling agent 3300, organic clay, organic pottery clay, gas phase titanium dioxide One or more in silicon, Tissuemat E and cellulose ether, more preferably anti-settling agent 3300, organic clay, organic pottery clay, gas Aerosil, Tissuemat E or cellulose ether, are particularly preferred as (Mo Nuolong) MONORAL 3300.
The addition of the defoamer is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art The proportioning of the conventional antifoam of material, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being adjusted, the addition of defoamer of the present invention is preferably 2~4 parts by weight, more preferably 2.2~3.8 Parts by weight, most preferably 2.5~3.5 parts by weight.
The specifically chosen of the defoamer is not particularly limited the present invention, with anti-corrosion well known to those skilled in the art Coating defoamer, those skilled in the art can be carried out according to practical situations, product requirement and quality requirement Selection and adjustment, defoamer of the present invention preferably include organosiloxane defoamer, polyether antifoam agent and dimethicone and disappeared One or more in infusion, 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 Conventional fillers proportioning, those skilled in the art can be according to practical situations, product requirement and quality requirement Selected and adjusted, the addition of filler of the present invention is preferably 20~40 parts by weight, more preferably 25~35 weight Part, most preferably 27~32 parts by weight.
The specifically chosen of the filler is not particularly limited the present invention, is applied with anti-corrosion well known to those skilled in the art Material 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 include oxide powder and zinc, ferrophosphorus powder, aluminum paste, mica powder, iron oxide red, calcium carbonate and One or more in talcum powder, more preferably oxide powder and zinc, ferrophosphorus powder, aluminum paste, mica powder, iron oxide red, heavy carbonic acid Two or more in calcium and talcum powder.
The addition of the graphene and the composite of zinc powder is not particularly limited the present invention, with art technology The proportioning of conventional zinc powder in anticorrosive paint known to personnel, those skilled in the art can be according to practical situations, production Product requirement and quality requirement are selected and adjusted, and the addition of the composite of graphene and zinc powder of the present invention is excellent Elect 220~280 parts by weight, most preferably more preferably 230~270 parts by weight, 240~260 parts by weight as.
Selection of the present invention to the zinc powder in the composite of the graphene and zinc powder is not particularly limited, with ability The selection of the conventional zinc powder of anticorrosive paint known to field technique personnel, those skilled in the art can be according to practical application Situation, product requirement and quality requirement are selected and adjusted, and the particle diameter of zinc powder of the present invention is preferably 0.1~200 μ M, more preferably 0.5~100 μm, most preferably more preferably 1~80 μm, 5~50 μm.
Definition of the present invention to the graphene in the composite of the graphene and zinc powder is not particularly limited, with this The definition of graphene known to art personnel, those skilled in the art can want according to practical situations, product Ask and quality requirement is selected and adjusted, graphene of the present invention is preferably the graphene of broad sense, i.e. graphite alkenes material Material, preferably includes the one or more in graphene, graphene oxide, redox graphene and modified graphene, more preferably For graphene, graphene oxide, redox graphene or modified graphene, most preferably graphene.
Specifically compound mode in the composite of the graphene and zinc powder is not particularly limited the present invention, with Compound mode well known to those skilled in the art, those skilled in the art can want according to practical situations, product Ask and quality requirement selected and adjusted, it is of the present invention it is compound preferably include to spray, smear brush, doping, growth, deposition, One or more in embedded, bonding, cladding and covering, more preferably spray, smear brush, doping, growth, deposition, embedded, viscous Close, coat or cover, most preferably coat or cover.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 zinc powder is preferably the zinc of the uniform composite graphite alkene in surface Powder material.
The present invention is not limited especially the specific ratio of graphene and zinc powder in the composite of the graphene and zinc powder System, with the ratio of graphene composite material well known to those skilled in the art, those skilled in the art can be according to reality Applicable cases, product requirement and quality requirement are selected and adjusted, the quality of graphene of the present invention and the zinc powder Than, or it can be preferably independently (0.01 that the graphene, which accounts for the ratio of the gross mass of the composite of the graphene and zinc powder, ~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 zinc powder is not particularly limited the present invention, with people in the art Usual sources known to member, commercially available purchase can also be prepared voluntarily, those skilled in the art can be according to reality Applicable cases, product requirement and quality requirement are selected and adjusted.
Above-mentioned steps of the present invention provide a kind of graphene/zinc powder composite, change the addition of graphite alkenes material Graphene and zinc powder, are combined by mode first, obtain the composite of graphene and zinc powder, are then combined again with other compositions Into anticorrosive paint.Selection and proportion optimizing of the present invention by composition, in conjunction with a variety of auxiliary agents, are applied more extensive Resin anti-corrosive paint.The resin anti-corrosive paint that the present invention is provided effectively solves ordinary graphite alkenes material and is difficult to ensure that It is even scattered, easily reunite and flexible inherent shortcoming；Although and improving the scattered of graphene by the way of addition dispersant Degree, but other impurities are readily incorporated, the drawbacks of can not also overcoming reunion；It also avoid in anticorrosive paint zinc content it is high with And the problem of film layer thickness.
Present invention also offers a kind of preparation method of resin anti-corrosive paint, it is characterised in that comprises the following steps：
A graphene and zinc powder) are obtained into the composite of graphene and zinc powder after first mixing；
B graphene and the composite of zinc powder, resin and the solvent for) obtaining above-mentioned steps are mixed, by again After rotary evaporation, 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 composite of graphene and zinc powder first by graphene and zinc powder.
The design parameter of the graphene is not particularly limited the present invention, with routine well known to those skilled in the art Graphite alkenes material parameter, those skilled in the art can be according to practical situations, product requirement and quality It is required that being selected and being 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 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 excellent Elect 1~100 μm as, more preferably 10~90 μm, more preferably 30~70 μm, more preferably 40~60 μm, be most preferably specifically 10~50 μm.
The present invention is to above-mentioned steps A), i.e. the specific preparation process of the composite of graphene and zinc powder is not limited especially System, with the blend step of graphene composite material well known to those skilled in the art, those skilled in the art can basis Practical condition, product requirement and quality requirement are selected and adjusted, and the present invention is combined to improve graphene/zinc powder The performance of material, optimized process flow and the integrality for ensureing process route, the step A) it is particularly preferred as
A1) by after graphene solution and zinc particle uniformly mixing, mixture is obtained；
A2) mixture for obtaining above-mentioned steps obtains the zinc powder of the dispersed graphene in surface after rotary evaporation Particle.
The particle diameter of the zinc powder is not particularly limited the present invention, with zinc particle well known to those skilled in the art Particle diameter, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement Whole, the particle diameter of zinc particle of the present invention is preferably 0.1~200 μm, more preferably 0.5~100 μm, more preferably 1~80 μm, most preferably 5~50 μm.
The concentration of the graphene solution is not particularly limited the present invention, with graphite well known to those skilled in the art The concentration of alkene solution, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement Selection and adjustment, the concentration of graphene solution of the present invention is preferably 0.01%~20%, and 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 well known to those skilled in the art The Conventional solvents of graphene solution, those skilled in the art can be according to practical condition, product requirement and quality It is required that selected and adjusted, the solvent of graphene solution of the present invention be preferably water, absolute ethyl alcohol, acetone, dimethylbenzene, One or more in n-butanol, espeleton, isopropanol and ethyl acetate, more preferably water, absolute ethyl alcohol, acetone, diformazan Benzene, n-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 stone after scattered Black 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 Process for dispersing, those skilled in the art can be selected according to practical condition, product requirement and quality requirement And adjustment, scattered preferably ultrasonic agitation processing of the present invention.
The consumption of the graphene solution and zinc particle is not particularly limited the present invention, with those skilled in the art Well known conventional ratio, those skilled in the art can enter according to practical condition, product requirement and quality requirement Row selection and adjustment, the mass ratio of graphene of the present invention and the zinc particle is preferably (0.01~1)：100, it is more excellent Elect as (0.05~0.8)：100, more preferably (0.08~0.7)：100, be most preferably (0.1~0.5)：100, specifically can be with For (0.2~0.4)：100.
The detailed process of the mixing is not particularly limited the present invention, is mixed with well known to those skilled in the art Journey, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement It is whole, to be uniformly mixed into preferred scheme, the specific steps of mixing of the present invention, i.e. step A1) be more specifically preferably：
Zinc particle is slowly added into the graphene solution after scattered, while uniform mixing, is mixed Thing.
The design parameter being slowly added to is not particularly limited the present invention, with well known to those skilled in the art slow Slowly the addition speed added, those skilled in the art can be according to practical condition, product requirement and quality requirement Selected and adjusted, 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 according to practical condition, product requirement and quality requirement, this The invention mixing preferably includes stirring mixing.
The design parameter of the stirring mixing is not particularly limited the present invention, with well known to those skilled in the art mixed The parameter of conjunction, 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 For 400~800rpm, most preferably more preferably 500~700rpm, 350~500rpm.
The mixture that then present invention obtains above-mentioned steps obtains the dispersed graphite in surface after rotary evaporation The zinc particle of alkene.
The present invention to above-mentioned steps A2) in rotary evaporation specific steps and parameter be not particularly limited, with this area skill The process and parameter of rotary evaporation known to art personnel, those skilled in the art can be according to practical condition, products It is required that and quality requirement selected and adjusted.
The rotating speed of the rotary evaporation is not particularly limited the present invention, is steamed with rotation well known to those skilled in the art The rotating speed of hair, those skilled in the art can be selected according to practical condition, product requirement and quality requirement And adjustment, the present invention is that preferably graphene and zinc particle are combined closely, and improves the dispersing uniformity of graphene, institute The rotary speed for stating 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, is steamed with rotation well known to those skilled in the art The temperature of hair, those skilled in the art can be selected according to practical condition, product requirement and quality requirement And adjustment, the present invention is that preferably graphene and zinc particle are combined closely, and improves the dispersing uniformity of graphene, institute The temperature for stating 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, is steamed with rotation well known to those skilled in the art The time of hair, those skilled in the art can be selected according to practical condition, product requirement and quality requirement And adjustment, the present invention is that preferably graphene and zinc particle are combined closely, and improves the dispersing uniformity of graphene, institute The time for stating rotary evaporation is preferably 0.5~1.5h, more preferably 0.7~1.3h, most preferably 0.9~1.1h, specifically can be with For loosely powdered is finally presented with the compound zinc particle by graphene.
The pressure of the rotary evaporation is not particularly limited the present invention, is steamed with rotation well known to those skilled in the art The pressure of hair, those skilled in the art can be selected according to practical condition, product requirement and quality requirement And adjustment, the present invention is that preferably graphene and zinc particle are combined closely, and improves the dispersing uniformity of graphene, institute The pressure for stating rotary evaporation is preferably less than equal to 0.1MPa, more preferably under tiny structure or vacuum condition, most preferably true Under empty 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 life Production situation, product requirement and quality requirement are selected and adjusted, and the equipment of rotary evaporation of the present invention is preferably revolving Evaporator.
The present invention further preferably employs rotary evaporation during the composite of graphene and zinc powder is prepared Technology, further preferably by controlling vacuum, rotary speed, revolving temperature (bath temperature) etc. to make graphene uniform be coated in zinc Powder particles surface, untill material is in drying regime, so that graphene, macroscopical or micron-sized zinc particle be combined closely Together, graphene dispersion problem of non-uniform can be effectively solved, its premium properties is preferably played, and can also obtain The zinc particle material of uniform graphene coated material, makes dispersed coating of the graphene to zinc particle become a reality.And And the present invention is special under conditions of existing without protective gas, carries out aforesaid operations, so that the production procedure simplified, life Produce equipment and reduce production consumption.Above-mentioned complex method technique that the present invention is provided is simple, mild condition, safety and environmental protection, It is more suitable for the big production of technology.
The present invention, by the dispersed encapsulated of graphene uniform on zinc particle surface, can obtain using the processing mode of revolving The graphene zinc particle that can uniformly coat, i.e., dispersed graphene.Graphene is not only fundamentally solved in solution The uneven disadvantage of middle mixing, ensure that the dispersed of graphene, and graphene is coated on into particle surface, can be with Ensure that its flat presentation of graphene reduces fold, preferably play its performance, asked so as to solve graphene dispersion well Topic, 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 zinc powder of the invention are mixed, After rotary evaporation again, mixture is obtained.
The mode of the mixing is not particularly limited the present invention, with the mixing of coating well known to those skilled in the art Mode, those skilled in the art can be selected and be adjusted according to practical condition, product requirement and quality requirement Whole, 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, with well known to those skilled in the art The mixed process and parameter of coating, those skilled in the art can be according to practical condition, product requirement and quality It is required that being selected and being adjusted, the specific steps and parameter of mixing of the present invention are preferably with reference to relevant national standard completion Can, the time of the mixing is preferably 0.5~2h, more preferably 0.7~1.8h, most preferably 1~1.5h, stone in the present invention The step of addition of black alkene does not influence mixing 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 ability The process and parameter of rotary evaporation known to field technique personnel, those skilled in the art can according to practical condition, Product requirement and quality requirement are selected and adjusted.
The rotating speed of the rotary evaporation again is not particularly limited the present invention, with rotation well known to those skilled in the art Turn the rotating speed of evaporation, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement Selection and adjustment, the present invention are improved preferably uniformly to mix the composite and other materials of graphene and zinc powder 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 again is not particularly limited the present invention, with rotation well known to those skilled in the art Turn the temperature of evaporation, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement Selection and adjustment, the present invention are improved preferably uniformly to mix the composite and other materials of graphene and zinc powder 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, most Preferably 67~72 DEG C.
The time of the rotary evaporation again is not particularly limited the present invention, with rotation well known to those skilled in the art Turn the time of evaporation, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement Selection and adjustment, the present invention are improved preferably uniformly to mix the composite and other materials of graphene and zinc powder with this The dispersing uniformity of graphene, the time of the rotary evaporation again is preferably 0.5~2h, more preferably 0.8~1.8h, most Preferably 1~1.5h.
The pressure of the rotary evaporation again is not particularly limited the present invention, with rotation well known to those skilled in the art Turn the pressure of evaporation, those skilled in the art can be carried out according to practical condition, product requirement and quality requirement Selection and adjustment, the present invention are improved preferably uniformly to mix the composite and other materials of graphene and zinc powder 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 life Production situation, product requirement and quality requirement are selected and adjusted, and the equipment of rotary evaporation of the present invention is preferably revolving Evaporator.
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 B) after preferably also include step C), i.e., described in again after rotary evaporation, in addition to step C)；The step C) it is preferably：After material and auxiliary agent after rotary evaporation again is mixed again, resin anti-corrosive paint is obtained.
The step C) can also further it be particularly preferred as：
C1 mixture, filler, dispersant, anti-settling agent and the defoamer for) obtaining above-mentioned steps by stirring mixing after, Obtain the first component of resin anti-corrosive paint；
By curing agent, accelerator and solvent after being again stirring for mixing, the second component of resin anti-corrosive paint is obtained.
The species of the auxiliary agent is not particularly limited the present invention, with Coatings Additives 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, Auxiliary agent of the present invention preferably includes coating itself (first component) used additives and (second component) used additives when coating is used, described First component used additives preferably include the one or more in dispersant, anti-settling agent, defoamer and filler, more preferably dispersant, It is a variety of in anti-settling agent, defoamer and filler；The second component used additives are preferably included in curing agent, accelerator and solvent It is a variety of in one or more, more preferably curing 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 1000~3000rpm, more preferably 1200~2700rpm, more preferably 1500~2500rpm, most preferably 1800 ~2200rpm.
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 1~3h, more excellent Elect 1.2~2.7h, most preferably 1.5~2.5h as.
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 1000~3000rpm, more preferably 1200~2700rpm, more preferably 1500~2500rpm, optimal Elect 1800~2200rpm as.
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 Situation, product requirement and quality requirement are selected and adjusted, it is of the present invention be again stirring for mixing time be preferably 0.5~2h, more preferably 0.8~1.8h, most preferably 1~1.5h.
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 Situation, product requirement and quality requirement are selected and adjusted, the temperature preferably room of the present invention for being again stirring for mixing Temperature, is specifically as follows 10~40 DEG C, can be 15~35 DEG C, or 20~30 DEG C.
The present invention changes traditional graphene addition manner, and graphene is wrapped in by chemistry or physics mode Zinc particle surface, is then used further in post-coatings production.And new dispersing mode is further preferably employed, can be from Fundamentally solve Flexible graphene and uneven disadvantage is mixed in coating system, ensure that the dispersed of graphene.Together When graphene is wrapped in zinc particle surface, it is ensured that its flat presentation of graphene reduces fold, preferably plays its property Energy.
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 zinc powder first Zinc particle after processing, is then added in anticorrosive paint by particle surface, and graphite alkenes material point can be solved well The problem of dissipating, it is ensured that the perfect performance of its premium properties；And other mixed and disorderly materials such as other dispersants need not be added, reduce The introducing of impurity, is effectively reduced negative effect of the pollutant to actual effect；The consumption of zinc powder is also greatly reduced, Production cost is not only greatly lowered, the zinc cigarette harm of human weld's process is also improved.The present invention is fundamentally solved Soft graphite alkenes material mixes uneven disadvantage in coating system, ensure that the dispersed of graphite alkenes material, Graphite alkenes material is wrapped in zinc particle surface simultaneously, it is ensured that graphene has preferable its flat presentation, reduces pleat Wrinkle, preferably plays its performance.
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 3000 hours, be 6 times of national standard, paint film structure and film thickness with high intensity The characteristics of thin, shock resistance is strong, can reach 120g.cm, and environment-friendly.
In order to further illustrate the present invention, a kind of 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 lower premised on technical solution of the present invention Implement, give detailed embodiment and specific operating process, simply to further illustrate the feature and excellent of the present invention Point, rather than limiting to the claimed invention, protection scope of the present invention are also not necessarily limited to following embodiments.
Embodiment 1
Graphene/zinc composite
1) it is 0.5% graphene ethanol solution, ultrasonic agitation 3h to take content；
2) 250g zinc powders are added slowly to step 1 under mechanical stirring according to the ratio of graphene 0.3%) in obtain Graphene solution in, persistently stir 30min；
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 zinc 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/zinc composite carries out macroscopic analysis, and zinc powder is relatively coated after coating Preceding obvious color burn.
The graphene prepared to above-mentioned steps of the present invention/zinc composite carries out transmission electron microscope micro-analysis, referring to Fig. 1, Fig. 1 is the TEM transmission electron microscope photos of graphene/zinc composite microscopic appearance prepared by the embodiment of the present invention 1.
Referring to Fig. 2, Fig. 2 is the TEM transmission electron microscope photos of common zinc particle microscopic appearance.
From Fig. 1 and 2, the present invention forms graphene film layer on zinc particle top layer, and the attachment of graphene film layer is equal It is even, agglomeration is had no, thickness is 10~60nm.
Resin anti-corrosive paint
1) take the above-mentioned contents of 250g for 0.3% graphene be modified zinc powder, 280g epoxy resin be dissolved in 200g dimethylbenzene with just Butanol 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 10g calcium carbonate, 10g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL 3300, high-speed stirred 30min, rotating speed 3000r/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 under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed and stir straight To being uniformly dispersed, second component is obtained.
8) anticorrosive paint in use, by the first and second components according to mass ratio 5:1 mixing.
Resin anti-corrosive paint prepared by the embodiment of the present invention 1 is detected.
Anticorrosive paint and the zinc-rich paint with formula prepared by above-mentioned steps, with electrolyte solution, polishing, cleaning electricity Pole；Then start instrument, preheat, open control software and assemble experimental provision again, after instrument state is normal, connecting wire；Choosing Measurement function is selected, it is 0mV to 2000mV, sweep speed to set electric potential scanning scope：100mV/s, measurement polarization curve carries out pole Change curve detection.
Referring to Fig. 3, Fig. 3 is the polarization of resin anti-corrosive paint and common zinc-rich anti-corrosive paint prepared by the embodiment of the present invention 1 Curve comparison figure.
From the figure 3, it may be seen that the corrosion current Icorr=6.8e-007A/cm of common zinc-rich paint2；And graphene coating Corrosion current Icorr=10.5e-011A/cm2, for common coating, corrosion current reduces by 3 orders of magnitude.
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 inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Embodiment 2
1) take the above-mentioned contents of 250g for 0.3% graphene be modified zinc powder, 250g epoxy resin be dissolved in 200g dimethylbenzene with just Butanol 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 10g calcium carbonate, 10g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL3300, high-speed stirred 30min, rotating speed 3000r/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 under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed and stir straight To being uniformly dispersed, second component is obtained.
8) anticorrosive paint in use, by the first and second components according to mass ratio 5:1 mixing.
Resin anti-corrosive paint prepared by the embodiment of the present invention 2 is detected.
Anticorrosive paint and the zinc-rich paint with formula prepared by above-mentioned steps, with reference to national standard《The zinc-rich bottoms of GB/T 3668 Paint standard》Carry out coating property detection.
Referring to Fig. 4, Fig. 4 is the cross-section structure of anticorrosive paint SEM ESEMs prepared by the embodiment of the present invention 2.Referring to Fig. 5, Fig. 5 are the cross-section structure of the SEM ESEMs of common zinc-rich anti-corrosive paint.
From Figure 4 and 5, the section structure zinc powder of common epoxy zinc-enriched paint is accumulated in a jumble, zinc powder and epoxy resin it Between wellability it is poor, there are a large amount of defects in resin solidification, and graphene modified anti-corrosive coating section is smooth, defect is few, and the degree of order is more Height, compactness is also more preferable.
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 inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Embodiment 3
1) take the above-mentioned contents of 250g for 0.3% graphene be modified zinc powder, 238g epoxy resin be dissolved in 200g dimethylbenzene with just Butanol 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 20g calcium carbonate, 20g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL3300, high-speed stirred 30min, rotating speed 3000r/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 under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed and stir straight To being uniformly dispersed, second component is obtained.
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 inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Embodiment 4
1) take the above-mentioned contents of 250g for 0.3% graphene be modified zinc powder, 222g epoxy resin be dissolved in 200g dimethylbenzene with just Butanol 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 20g calcium carbonate, 20g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL 3300, high-speed stirred 30min, rotating speed 3000r/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 under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed and stir straight To being uniformly dispersed, second component is obtained.
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 4.
Referring to table 1, the paint film property inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Embodiment 5
1) take the above-mentioned contents of 250g for 0.3% graphene be modified zinc powder, 208g epoxy resin be dissolved in 200g dimethylbenzene with just Butanol 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 30g calcium carbonate, 30g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL 3300, high-speed stirred 30min, rotating speed 3000r/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 under DMP-30 1g, polyamide 200 25g, 1000r/min rotating speed and stir straight To being uniformly dispersed, second component is obtained.
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 5.
Referring to table 1, the paint film property inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Comparative example 1
1) 250g zinc powders, 208g epoxy resin is taken to be dissolved in 200g dimethylbenzene and n-butanol with 3:The mixed solvent of 1 mixing In, 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 10g calcium carbonate, 10g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL 3300, high-speed stirred 30min, rotating speed 3000r/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 and stirred under DMP-30 1g, polyamide 200 25g, 700~1500r/min rotating speed Mix up to being uniformly dispersed, obtain 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 common zinc-rich anti-corrosive paint prepared by above-mentioned steps.
Referring to table 1, the paint film property inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Comparative example 2
1) 250g zinc powders, 222g epoxy resin is taken to be dissolved in 200g dimethylbenzene and n-butanol with 3:The mixed solvent of 1 mixing In, 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 20g calcium carbonate, 20g ferrophosphorus Powder, 1.4g propene carbonates, 12g aluminum pastes, 3g defoamers, 2.4g MONORAL 3300, high-speed stirred 30min, rotating speed 3000r/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 and stirred under DMP-30 1g, polyamide 200 25g, 700~1500r/min rotating speed Mix up to being uniformly dispersed, obtain 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 common zinc-rich anti-corrosive paint prepared by above-mentioned steps.
Referring to table 1, the paint film property inspection of resin anti-corrosive paint and common zinc-rich anti-corrosive paint that table 1 is prepared for the present invention Survey.
Table 1
A kind of resin anti-corrosive paint containing graphite alkenes/zinc powder composite and its system provided above the present invention Preparation Method is described in detail, and specific case used herein is explained the principle and embodiment of the present invention State, 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 the present invention On the premise of principle, 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 It is required that protection domain in.The scope of patent protection of the present invention is defined by the claims, and may include art technology Personnel it is conceivable that other embodiment.If these other embodiments, which have, is not different from claim character express Structural element, or if they include equivalent structural elements of the character express without essence difference with claim, then this A little other embodiments 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 the composite and solvent of resin, graphene and zinc powder.
2. resin anti-corrosive paint according to claim 1, it is characterised in that the resin is 230~330 parts by weight；
The composite of graphene and zinc powder is 220~280 parts by weight；
Solvent is 176~236 parts by weight；
The resin anti-corrosive paint also includes auxiliary agent.
3. resin anti-corrosive paint according to claim 2, it is characterised in that the auxiliary agent includes curing agent, accelerator, divided One or more in powder, anti-settling agent, defoamer and filler；
The curing agent is 2~8 parts by weight；
The dispersant is 1~2 parts by weight；
The accelerator is 0.1~0.4 parts by weight；
The anti-settling agent is 2~3 parts by weight；
The defoamer is 2~4 parts by weight；
The filler is 20~40 parts by weight.
4. resin anti-corrosive paint according to claim 3, it is characterised in that the composite of the graphene and zinc powder is The zinc powder 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 dispersant includes propene carbonate, Tissuemat E, polyacrylic acid sodium salt, styrene-maleic acid half ester compound, benzene second Alkene acrylic copolymer, acrylic acrylate copolymer, polyvinylpyrrolidone, polyurethane, polyethylene glycol and polyvinyl alcohol In one or more；
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 zinc powder) are obtained into the composite of graphene and zinc powder after first mixing；
B graphene and the composite of zinc powder, resin and the solvent for) obtaining above-mentioned steps are mixed, by rotating again After evaporation, 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 zinc powder uniformly mixing, mixture is obtained；
A2) mixture for obtaining above-mentioned steps is after rotary evaporation, obtain the dispersed graphene in surface graphene and Zinc powder composite.
7. preparation method according to claim 6, it is characterised in that the mass ratio of the graphene and the zinc powder is (0.01~1)：100；
The step A2) 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 0.5~1.5h.
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；
The step B) also include step C afterwards)；
C after) material and auxiliary agent after rotary evaporation again are mixed again, resin anti-corrosive paint is obtained.
9. the preparation method according to claim 8 any one, it is characterised in that the step C) be specially：
C1) material after rotary evaporation again, filler, dispersant, anti-settling agent and defoamer are obtained after stirring mixing To the first component of resin anti-corrosive 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, dispersant, 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~ 3000rpm；The time of the stirring mixing is 1~3h；
The rotating speed for being again stirring for mixing is 1000~3000rpm；The time for being again stirring for mixing is 0.5~2h.
CN201710292674.7A 2017-04-28 2017-04-28 A kind of resin anti-corrosive paint containing graphene/zinc powder composite and preparation method thereof Pending CN107099217A (en)

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