CN105778716A - Preparation method for graphene modified anticorrosive paint - Google Patents
Preparation method for graphene modified anticorrosive paint Download PDFInfo
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- 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
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/04—Condensation polymers of aldehydes or ketones with phenols only
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/10—Epoxy resins modified by unsaturated compounds
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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- 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
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
The invention discloses a preparation method for graphene modified anticorrosive paint. The preparation method comprises the following steps: (1) adding resin into a solvent to dissolve, adding a stabilizer and graphene powder into the resin after the resin is dissolved, uniformly mixing, and treating by adopting a dispersing process, thereby obtaining graphene-resin composite slurry; (2) additionally getting resin to mix with the solvent and a filler to obtain a mixture, adding a dispersing agent into the uniformly-mixed mixture, and treating by adopting a dispersing process, thereby obtaining color paste, wherein the type of the additionally-got resin is the same as that of the resin in the step (1); and (3) adding the color paste prepared in the step (2) into the graphene-resin composite slurry prepared in the step (1), and filtering after grinding and dispersing, thereby obtaining the finished paint. According to the preparation method, a path of adding a corrosive medium to protected matrix is added, so that the protection time of a coating on the matrix is prolonged, and the purpose of long-acting corrosion prevention is achieved; and the defects of poor weather resistance, low barrier property, short service life and the like of the current paint are overcome.
Description
Technical field
The present invention relates to anticorrosive paint field, the preparation method relating in particular to a kind of Graphene modified anti-corrosive coating.
Background technology
Existing anticorrosive paint kind is more, incomplete statistics, China's anticorrosive paint kind has kind more than 1000, and traditional has epoxy, bituminous epoxy, Colophonium, chlorinated rubber, chlorosulfonated polyethylene, polrvinyl chloride, Vinylidene Chloride, cashew resin, silester, highly-chlorinated polyethylene, polyurethane, polyurethane asphalt, phenolic aldehyde, alkyd paint etc. by resin classification.And epoxy resin anticorrosive paint is a topmost class in anticorrosive paint.Epoxy resin anticorrosive paint specifically includes that epoxy zinc-rich corrosion resistant coating, epoxy coal asphalt paint, epoxy glass flake paint and powder epoxy corrosion resistant coating and emulsion type epoxy anticorrosive paint.Existing anticorrosive additive is mainly metal dust (such as zinc powder) and glass flake, is all relatively larger granule, and consumption is very big, and manufacturability and property easy to use impact on coating are very big.
In order to solve above-mentioned technical problem, prior art proposes in anticorrosive paint, adds the technology that coating is modified by Graphene, as China Patent No. " 201410480336.2 " discloses " toner coating that a kind of Graphene is modified and production technology " on the 10th at December in 2014, the toner coating that its technical scheme is described includes resin, filler, auxiliary agent, pigment and Graphene；Mass percent is as follows: resin: 50%-80%；Filler: 0%-40%；Auxiliary agent: 5%-7%；Pigment: 0.2%-3%；Graphene: 0.005 30%.Its preparation technology comprises the steps: (1), ratio described in claim 1 of resin, firming agent, auxiliary agent, pigment and Graphene put in high speed mixer and mix；(2), then this mixture is melted in the batch mixer of high-temperature heating；(3), being melted into slurry like material and extruded by screw machine, roll-in is in blocks, and cooling makes mixture solidify, and is pressed into sheet stock subsequently；(4), then by sheet stock thing grinding to form particulate powder by gradation and lock out operation, its particle diameter is 10 100 μm, makes toner coating.But this patent is in actual application, yet suffer from following defect: one, when the addition of Graphene is 30%, the consumption of Graphene is excessive, cause high cost, and the membership that adds of a large amount of Graphene affects the mechanical performance of coating, such as toughness, intensity, cause mechanical properties decrease after curing of coatings；It addition, Graphene is as high conductive material, adds membership in a large number and make corrosion-inhibiting coating have electric conductivity, be unfavorable for being used in oil and gas pipes and other special dimensions.And when Graphene addition is 0.005%, Graphene effect in the coating is very little, Graphene can not reach desirable dispersity (the staggered tiling overlap joint of each lamella, intercept corrosive medium) in system, and the antiseptic effect ultimately resulting in product is poor.Two, this patent needs high-temperature heating in preparation process, and production technology is complex, and manufacturing cost is higher, and, the coating that the method is produced is powdery paints, and the scope of application is less.
Summary of the invention
It is an object of the invention to solve the above-mentioned problems in the prior art; the preparation method that a kind of Graphene modified anti-corrosive coating is provided; invention increases corrosive medium and arrive the path of protection matrix; thus extending the coating guard time to matrix; reach the purpose of long-effective corrosion, and overcome that existing coating weatherability is poor, barrier is low and the defect such as service life is short.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of a kind of Graphene modified anti-corrosive coating, it is characterised in that comprise the following steps:
(1) Graphene resin compounded slurry, is prepared
Resin is joined in solvent and dissolve, dissolve and backward resin adds stabilizer and graphene powder, after mix homogeneously, adopt dispersing technology to process, obtain Graphene resin compounded slurry；
(2), preparation mill base
Separately take resin, solvent mixes with filler, adds dispersant, then adopts dispersing technology to process, obtain mill base after mix homogeneously；Wherein, the resinous type separately taken is identical with the resinous type in step (1)；
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion is filtered after processing, and namely obtains finished product coating.
In described step (1), resin is joined in solvent and dissolve, after uniform dissolution, be initially charged stabilizer mix homogeneously, add graphene powder mix homogeneously, finally adopt dispersing technology to process 0.5 1.5h, obtain Graphene resin compounded slurry.
In described step (2), first separately take resin and be mixed and stirred for uniformly with solvent, under stirring, then add filler, after filler mix homogeneously, add dispersant, then adopt dispersing technology to process 1.5 2.5h, obtain mill base.
In described step (3), being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling disperses 45 75min, filtration treatment after stopping dispersion, namely obtains the finished product coating of Dark grey.
In described step (1), resin is 50 70:30 50 with the mass ratio of solvent, and the mass ratio of resin and stabilizer is 100:1 1.5, and the mass ratio of resin and graphene powder is 98 98.8:1.2 2.
Graphene powder in described step (1) should carry out pre-dispersed process before addition, the concrete technique that processes is: is placed in by graphene powder in the solvent described in step (1) and disperses 20 40min with ultrasonic echography, after having disperseed, remove solvent by filter cloth order number vacuum filtration machine more than 500 orders, obtain moistening Graphene；Wherein, graphene powder is 1:250 300 with the mass ratio of solvent.
Stabilizer in described step (1) is one or both the mixing in polyvinylpyrrolidone, silane coupler.
In described step (2), resin is 60 70:5 25:7 35 than solvent than the mass ratio of filler.
Filler in described step (2) is titanium dioxide, Pulvis Talci, mica sheet or iron oxide red.
In described step (3), before sand milling dispersion processes, Graphene resin compounded slurry is added with in anti-flooding assistant, anti-settling agent, anti-sagging agent, levelling agent, defoamer one or more；When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5 1.0% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent or anti-sagging agent, the addition of anti-settling agent or anti-sagging agent is the 1 2% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent or defoamer, the addition of levelling agent or defoamer is the 1 1.5% of mill base and Graphene resin compounded slurry gross mass.
Described resin is epoxy resin, alkyd resin, acrylic resin, epoxy modified silicone resin, phenolic resin or vinylite, when resin is solid-state, needs before use to smash into solid resin to pieces powder；Described solvent is dehydrated alcohol, dimethylbenzene, n-butyl alcohol, Ketohexamethylene, methyl iso-butyl ketone (MIBK) one or more mixing therein.
Described dispersing technology is high speed magnetic stirring technique, emulsification pretreatment dispersing technology, high speed homogenization dispersed with stirring technique, ball-milling method dispersing technology or sand milling dispersing technology.
Employing it is an advantage of the current invention that:
One, in the present invention; Graphene is as a kind of hypotonicity, flake additive; by Graphene, coating is modified; the main composite coating based on physical isolation anticorrosion can be obtained; this composite coating has the characteristics such as adhesive force is strong, intensity is high, high barrier, anti-ion permeability strong, resistant to chemical media corrosivity is strong; can the infiltration of effectively blocking oxygen, ion and hydrone so that protected matrix material will not touch corrosive medium, thus avoiding or suppress the corrosion of material.Additionally; the present invention adopts the coating that above-mentioned specific preparation technology, component and parameter prepare; there is the excellent properties that can extend corrosive medium arrival protection matrix path; and then the coating guard time to matrix can be extended; reach the purpose of long-effective corrosion, and overcome that existing coating weatherability is poor, barrier is low and the defect such as service life is short.
Two, in the present invention, graphene powder has very high chemical inertness and higher surface can, very easily there is agglomeration in a solvent, so at graphene powder before joining in resin, it being carried out pretreatment and can effectively prevent Graphene from reuniting in resin.
Three, in the present invention, painting color can be made uniform by anti-flooding assistant, it is to avoid floating phenomenon occurs.By anti-settling agent, anti-sagging agent, levelling agent and defoamer, the stability of coating can be improved, be conducive to extending the time of coating protection matrix.
Four, the graphene powder addition in the present invention is less, compared to the addition of metal zinc 60 80%wt and the addition of glass Microsheet 10 30wt% in epoxy glass flake paint in prior art epoxy zinc rich primer, in Graphene modified anti-corrosive coating, the addition of graphene powder is less than 1.0wt%, substantially without the application process and the scope of application that change existing coating.Again due to the chemical inertness of Graphene self with to organic molecule affinity so that it is can be added in the matrixes such as most of coating, resin, plastics, without destroying the chemical property of matrix, the rheological equationm of state etc..Can be widely used for the anticorrosion engineering in various acid, alkali, salt, the wet goods corrosive environments such as soil, air, seashore, sea water, and at antiseptic projects such as empty space flight, Hai Gong, boats and ships, container, electronics, petrochemical industry, wind-powered electricity generation, the energy, municipal works, there is broad prospect of application, be a kind of novel anti-corrosion material.Additionally, the present invention need not heat in preparation process, resin uses solvent to dissolve, and has that production technology is simple, production cost is low and the advantage such as good product performance.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Resin is proportionally added in solvent and dissolves, in resin, stabilizer and graphene powder is added in proportion after uniform dissolution, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes the solvent of classification as hereinbefore and is placed in by graphene powder in this solvent, the mass ratio of graphene powder and solvent is 1:250 300, then 20 40min are disperseed with ultrasonic echography, after having disperseed, solvent is removed by filter cloth order number vacuum filtration machine more than 500 orders, obtain moistening Graphene, again lubricating graphite alkene is joined in resin, the mode then passing through stirring makes stabilizer, Graphene and mixed with resin are uniform, after mix homogeneously, dispersing technology is adopted to process 0.5 1.5h, process obtains Graphene resin compounded slurry after completing.Wherein, the mass ratio of resin and solvent is 50 70:30 50, and the mass ratio of resin and stabilizer is 100:1 1.5, and the mass ratio of resin and graphene powder is 98 98.8:1.2 2.
In the present embodiment, described stabilizer is one or both the mixing in polyvinylpyrrolidone, silane coupler.Wherein, owing to polyvinylpyrrolidone is solid matter, therefore when using polyvinylpyrrolidone, dehydrated alcohol must be added in polyvinylpyrrolidone, form the ethanol solution of polyvinylpyrrolidone, and silane coupler is KH560, for liquid, can directly use.
Described resin is epoxy resin, alkyd resin, acrylic resin, epoxy modified silicone resin, phenolic resin or vinylite, when resin is solid-state, needing to smash into solid resin to pieces powder before use, the size of powder is not intended to, it is possible to rapid solution is in solvent；Described solvent is dehydrated alcohol, dimethylbenzene, n-butyl alcohol, Ketohexamethylene one or more mixing therein.Wherein, solvent is consubstantiality series solvent, when using multi-solvents, multi-solvents can mixing, mutually do not react, and not in resin reaction.
In the present embodiment, described dispersing technology is high speed magnetic stirring technique, emulsification pretreatment dispersing technology, high speed homogenization dispersed with stirring technique, ball-milling method dispersing technology or sand milling dispersing technology.
(2), preparation mill base
Separately take resin, solvent mixes by the mass ratio of 60 70:5 25:7 35 with filler, adds dispersant, then adopts any one dispersing technology above-mentioned to process 1.5 2.5h, obtain mill base after having processed after mix homogeneously；Wherein, described filler is the inorganic fillers such as titanium dioxide, Pulvis Talci, mica sheet or iron oxide red, and the resinous type separately taken is identical with the resinous type in step (1), and the solvent separately taken can be identical with the solvent in step (1).
(3), modulation coating
Mill base obtained in step (2) is joined in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 45 75min, adopting spin vibration sieve filtration treatment after stopping dispersion, sieve number is 200 500 orders, namely obtains finished product coating after filtration treatment.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant, in order to improve the stability of coating, Graphene resin compounded slurry is added with one or more in anti-settling agent, anti-sagging agent, levelling agent, defoamer；When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5 1.0% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent or anti-sagging agent, the addition of anti-settling agent or anti-sagging agent is the 1 2% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent or defoamer, the addition of levelling agent or defoamer is the 1 1.5% of mill base and Graphene resin compounded slurry gross mass.
Embodiment 2
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Epoxy resin is proportionally added in dehydrated alcohol, and adopt the mode of stirring to make epoxy resin uniform dissolution, to reduce the viscosity of epoxy resin, the mass ratio of epoxy resin and dehydrated alcohol is 70:30, after uniform dissolution, in epoxy resin, first add polyvinylpyrrolidone in proportion and be uniformly mixed, the mass ratio of epoxy resin and polyvinylpyrrolidone is 100:1, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of epoxy resin and graphene powder is 98.8:1.2, after mix homogeneously to be mixed, emulsification pretreatment dispersing technology dispersion is adopted to process 0.5h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes dehydrated alcohol and is placed in by graphene powder in this dehydrated alcohol, the mass ratio of graphene powder and dehydrated alcohol is 1:250, then disperse 20min with ultrasonic echography, after ultrasonic disperse completes, remove dehydrated alcohol by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the epoxy resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First another extracting epoxy resin is mixed and stirred for uniformly with dehydrated alcohol, reduce the viscosity of epoxy resin, it is subsequently adding titanium dioxide, add while stirring, it is generally required to 30min can add, after titanium dioxide mix homogeneously, add dispersant, then adopt emulsification pretreatment dispersing technology to process 1.5h with the rotating speed dispersion of 8000rpm/min, obtain mill base.Wherein, epoxy resin, dehydrated alcohol mix by the mass ratio of 60:5:35 with titanium dioxide.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 45min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with anti-settling agent, anti-flooding assistant and anti-settling agent all add before sand milling dispersion processes, and anti-settling agent is generally adopted aerosil etc..When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent, the addition of anti-settling agent is the 1% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 3
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Alkyd resin is proportionally added in dimethylbenzene, and adopt the mode of stirring to make alkyd resin uniform dissolution, to reduce the viscosity of alkyd resin, the mass ratio of alkyd resin and dimethylbenzene is 65:35, after uniform dissolution, in alkyd resin, first add silane coupler in proportion and be uniformly mixed, the mass ratio of alkyd resin and silane coupler is 100:1.5, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of alkyd resin and graphene powder is 98:2, after mix homogeneously to be mixed, high speed homogenization dispersed with stirring technique dispersion is adopted to process 1.5h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes diformazan benzo and is placed in by graphene powder in this dimethylbenzene, the mass ratio of graphene powder and dimethylbenzene is 1:300, then disperse 40min with ultrasonic echography, after having disperseed, remove dimethylbenzene by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the alkyd resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First separately take alkyd resin and be mixed and stirred for uniformly with dimethylbenzene, reduce the viscosity of alkyd resin, it is subsequently adding Pulvis Talci, add while stirring, it is generally required to 60min can add, after Pulvis Talci mix homogeneously, add dispersant, then adopt high speed homogenization dispersed with stirring technique dispersion to process 2.5h, obtain mill base.Wherein, alkyd resin, dimethylbenzene mix by the mass ratio of 60:25:15 with Pulvis Talci.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 75min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with anti-settling agent and anti-sagging agent two kinds, anti-flooding assistant, anti-settling agent and anti-sagging agent all add before sand milling dispersion processes, and anti-settling agent and anti-sagging agent are generally adopted organobentonite etc..When adding anti-flooding assistant, the addition of anti-flooding assistant is the 1.0% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent and anti-sagging agent, the addition of anti-settling agent and anti-sagging agent is the 2% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 4
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Acrylic resin is proportionally added in dimethylbenzene, and adopt the mode of stirring to make acrylic resin uniform dissolution, to reduce the viscosity of acrylic resin, the mass ratio of acrylic resin and dimethylbenzene is 60:40, after uniform dissolution, first in acrylic resin, add the stabilizer mixed by polyvinylpyrrolidone and silane coupler in proportion, and be uniformly mixed, the mass ratio of acrylic resin and stabilizer is 100:1.2, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of acrylic resin and graphene powder is 98.5:1.5, after mix homogeneously to be mixed, ball-milling method dispersing technology dispersion is adopted to process 1h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes diformazan benzo and is placed in by graphene powder in this dimethylbenzene, the mass ratio of graphene powder and dimethylbenzene is 1:280, then disperse 30min with ultrasonic echography, after having disperseed, remove dimethylbenzene by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the acrylic resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First separately take acrylic resin and be mixed and stirred for uniformly with dimethylbenzene, reduce the viscosity of acrylic resin, it is subsequently adding titanium dioxide, add while stirring, it is generally required to 40min can add, after titanium dioxide mix homogeneously, add dispersant, then adopt ball-milling method dispersing technology dispersion to process 2h, obtain mill base.Wherein, acrylic resin, dimethylbenzene mix by the mass ratio of 70:23:7 with titanium dioxide.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 60min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with anti-settling agent, anti-sagging agent, levelling agent and defoamer four kinds, anti-flooding assistant, anti-settling agent, anti-sagging agent, levelling agent and defoamer all add before sand milling dispersion processes, and anti-settling agent and anti-sagging agent are generally adopted aerosil etc., levelling agent and defoamer and buy in market.When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.7% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent and anti-sagging agent, the addition of anti-settling agent and anti-sagging agent is the 1.5% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent and defoamer, the addition of levelling agent and defoamer is the 1% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 5
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Epoxy modified silicone resin is proportionally added in Ketohexamethylene, and adopt the mode of stirring to make epoxy modified silicone resin uniform dissolution, to reduce the viscosity of epoxy modified silicone resin, the mass ratio of epoxy modified silicone resin and Ketohexamethylene is 55:45, after uniform dissolution, in epoxy modified silicone resin, first add silane coupler in proportion and be uniformly mixed, the mass ratio of epoxy modified silicone resin and silane coupler is 100:1.4, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of epoxy modified silicone resin and graphene powder is 98.2:1.8, after mix homogeneously to be mixed, emulsification pretreatment dispersing technology dispersion is adopted to process 0.5h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes Ketohexamethylene and is placed in by graphene powder in this Ketohexamethylene, the mass ratio of graphene powder and Ketohexamethylene is 1:260, then disperse 25min with ultrasonic echography, after having disperseed, remove Ketohexamethylene by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the epoxy modified silicone resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First separately take epoxy modified silicone resin and be mixed and stirred for uniformly with Ketohexamethylene, reduce the viscosity of epoxy modified silicone resin, it is subsequently adding Pulvis Talci, add while stirring, it is generally required to 50min can add, after Pulvis Talci mix homogeneously, add dispersant, then adopt emulsification pretreatment dispersing technology dispersion to process 1.5h, obtain mill base.Wherein, epoxy modified silicone resin, Ketohexamethylene mix by the mass ratio of 65:20:15 with Pulvis Talci.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 50min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with anti-settling agent and levelling agent two kinds, anti-flooding assistant, anti-settling agent and levelling agent all add before sand milling dispersion processes, and anti-settling agent is generally adopted aerosil etc., and levelling agent is bought in market.When adding anti-flooding assistant, the addition of anti-flooding assistant is the 1.0% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent, the addition of anti-settling agent is the 1% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent, the addition of levelling agent is the 1.5% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 6
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Phenolic resin is proportionally added in dehydrated alcohol, and adopt the mode of stirring to make phenolic resin uniform dissolution, to reduce the viscosity of phenolic resin, the mass ratio of phenolic resin and dehydrated alcohol is 65:35, after uniform dissolution, in phenolic resin, first add polyvinylpyrrolidone in proportion and be uniformly mixed, the mass ratio of phenolic resin and polyvinylpyrrolidone is 100:1.2, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of phenolic resin and graphene powder is 98:2, after mix homogeneously to be mixed, ball-milling method dispersing technology dispersion is adopted to process 1.5h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes dehydrated alcohol and is placed in dehydrated alcohol by graphene powder, the mass ratio of graphene powder and dehydrated alcohol is 1:300, then disperse 25min with ultrasonic echography, after having disperseed, remove dehydrated alcohol by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the phenolic resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First separately take phenolic resin and be mixed and stirred for uniformly with dehydrated alcohol, reduce the viscosity of phenolic resin, it is subsequently adding Pulvis Talci, add while stirring, it is generally required to 30min can add, after Pulvis Talci mix homogeneously, add dispersant, then adopt ball-milling method dispersing technology dispersion to process 1.5h, obtain mill base.Wherein, phenolic resin, dehydrated alcohol mix by the mass ratio of 70:15:15 with Pulvis Talci.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 55min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with defoamer, anti-flooding assistant and defoamer all add before sand milling dispersion processes, and defoamer is bought in market.When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5% of mill base and Graphene resin compounded slurry gross mass；When adding defoamer, the addition of defoamer is the 1.2% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 7
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Vinylite is proportionally added in the solvent mixed with dimethylbenzene by dehydrated alcohol, and adopt the mode of stirring to make vinylite uniform dissolution, to reduce the viscosity of vinylite, the mass ratio of vinylite and solvent is 58:42, after uniform dissolution, in vinylite, first add polyvinylpyrrolidone in proportion and be uniformly mixed, the mass ratio of vinylite and polyvinylpyrrolidone is 100:1.5, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of vinylite and graphene powder is 98.4:1.6, after mix homogeneously to be mixed, emulsification pretreatment dispersing technology dispersion is adopted to process 1.5h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes the solvent mixed with dimethylbenzene by dehydrated alcohol and is placed in by graphene powder in this solvent, the mass ratio of graphene powder and solvent is 1:260, then disperse 35min with ultrasonic echography, after having disperseed, remove solvent by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the vinylite after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First separately take vinylite and be mixed and stirred for uniformly with the solvent mixed with dimethylbenzene by dehydrated alcohol, reduce the viscosity of vinylite, it is subsequently adding Pulvis Talci, add while stirring, it is generally required to 40min can add, after Pulvis Talci mix homogeneously, add dispersant, then adopt emulsification pretreatment dispersing technology dispersion to process 1.5h, obtain mill base.Wherein, vinylite, dehydrated alcohol mix by the mass ratio of 70:5:25 with Pulvis Talci.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 50min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with levelling agent, anti-flooding assistant and levelling agent all add before sand milling dispersion processes, and levelling agent is bought in market.When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.7% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent, the addition of levelling agent is the 1.3% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Embodiment 8
The preparation method of a kind of Graphene modified anti-corrosive coating, comprises the following steps:
(1) Graphene resin compounded slurry, is prepared
Epoxy resin is proportionally added in dimethylbenzene, and adopt the mode of stirring to make epoxy resin uniform dissolution, to reduce the viscosity of epoxy resin, the mass ratio of epoxy resin and dimethylbenzene is 60:40, after uniform dissolution, in epoxy resin, first add polyvinylpyrrolidone in proportion and be uniformly mixed, the mass ratio of epoxy resin and polyvinylpyrrolidone is 100:1, it is proportionally added into graphene powder again and is uniformly mixed, the mass ratio of epoxy resin and graphene powder is 98.8:1.2, after mix homogeneously to be mixed, emulsification pretreatment dispersing technology dispersion is adopted to process 1h again, process obtains Graphene resin compounded slurry after completing.Wherein, graphene powder should carry out pre-dispersed process before addition, the concrete technique that processes is: separately takes dehydrated alcohol and is placed in by graphene powder in this dehydrated alcohol, the mass ratio of graphene powder and dehydrated alcohol is 1:250, then disperse 20min with ultrasonic echography, after ultrasonic disperse completes, remove dehydrated alcohol by filter cloth order number vacuum filtration machine more than 500 orders, obtaining moistening Graphene, graphene powder joins in the epoxy resin after dissolving with the state of lubricating graphite alkene.
(2), preparation mill base
First another extracting epoxy resin is mixed and stirred for uniformly with dimethylbenzene, reduce the viscosity of epoxy resin, it is subsequently adding iron oxide red, add while stirring, it is generally required to 30min can add, after iron oxide red mix homogeneously, add dispersant, then adopt emulsification pretreatment dispersing technology to process 1.5h with the rotating speed dispersion of 8000rpm/min, obtain mill base.Wherein, epoxy resin, dimethylbenzene mix by the mass ratio of 60:10:30 with iron oxide red.
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion processes 45min, stops filtration treatment after sand milling disperses, namely obtains the finished product coating of Dark grey after having filtered.Wherein, in order to avoid floating phenomenon occurs in coating, Graphene resin compounded slurry is added with anti-flooding assistant BYK-104S etc., in order to improve the stability of coating, Graphene resin compounded slurry is added with anti-settling agent, anti-flooding assistant and anti-settling agent all add before sand milling dispersion processes, and anti-settling agent is generally adopted aerosil etc..When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent, the addition of anti-settling agent is the 1% of mill base and Graphene resin compounded slurry gross mass.
(4), filter, canned
It is filtered gained finished product coating in step (3) processing, elimination big particle, tinning finished product.
Present invention existing coating testing standard or industry standard or international standard have carried out a large amount of dependence test, through experimental results demonstrate, this is implemented you and also adopts specific component and specific parameter, can preparing the coating with excellent antiseptic property, following table is the performance parameter of the coating adopting the method for the present embodiment to prepare:
Claims (10)
1. the preparation method of a Graphene modified anti-corrosive coating, it is characterised in that comprise the following steps:
(1) Graphene resin compounded slurry, is prepared
Resin is joined in solvent and dissolve, dissolve and backward resin adds stabilizer and graphene powder, after mix homogeneously, adopt dispersing technology to process, obtain Graphene resin compounded slurry；
(2), preparation mill base
Separately take resin, solvent mixes with filler, adds dispersant, then adopts dispersing technology to process, obtain mill base after mix homogeneously；Wherein, the resinous type separately taken is identical with the resinous type in step (1)；
(3), modulation coating
Being joined by mill base obtained in step (2) in Graphene resin compounded slurry obtained in step (1), sand milling dispersion is filtered after processing, and namely obtains finished product coating.
2. the preparation method of a kind of Graphene modified anti-corrosive coating as claimed in claim 1, it is characterized in that: in described step (1), resin is joined in solvent and dissolve, after uniform dissolution, it is initially charged stabilizer mix homogeneously, add graphene powder mix homogeneously, finally adopt dispersing technology to process 0.5 1.5h, obtain Graphene resin compounded slurry.
3. the preparation method of a kind of Graphene modified anti-corrosive coating as claimed in claim 1, it is characterized in that: in described step (2), first separately take resin and be mixed and stirred for uniformly with solvent, then under stirring, add filler, dispersant is added after filler mix homogeneously, adopt dispersing technology to process 1.5 2.5h again, obtain mill base.
4. the preparation method of a kind of Graphene modified anti-corrosive coating as claimed in claim 1, it is characterized in that: in described step (3), mill base obtained in step (2) is joined in Graphene resin compounded slurry obtained in step (1), sand milling disperses 45 75min, filtration treatment after stopping dispersion, namely obtains the finished product coating of Dark grey.
5. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterized in that: in described step (1), resin is 50 70:30 50 with the mass ratio of solvent, the mass ratio of resin and stabilizer is 100:1 1.5, and the mass ratio of resin and graphene powder is 98 98.8:1.2 2.
6. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterized in that: the graphene powder in described step (1) should carry out pre-dispersed process before addition, the concrete technique that processes is: is placed in by graphene powder in the solvent described in step (1) and disperses 20 40min with ultrasonic echography, after having disperseed, remove solvent by filter cloth order number vacuum filtration machine more than 500 orders, obtain moistening Graphene；Wherein, graphene powder is 1:250 300 with the mass ratio of solvent.
7. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterised in that: in described step (2), resin is 60 70:5 25:7 35 than solvent than the mass ratio of filler.
8. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterized in that: in described step (3), before sand milling dispersion processes, Graphene resin compounded slurry is added with in anti-flooding assistant, anti-settling agent, anti-sagging agent, levelling agent, defoamer one or more；When adding anti-flooding assistant, the addition of anti-flooding assistant is the 0.5 1.0% of mill base and Graphene resin compounded slurry gross mass；When adding anti-settling agent or anti-sagging agent, the addition of anti-settling agent or anti-sagging agent is the 1 2% of mill base and Graphene resin compounded slurry gross mass；When adding levelling agent or defoamer, the addition of levelling agent or defoamer is the 1 1.5% of mill base and Graphene resin compounded slurry gross mass.
9. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterized in that: described resin is epoxy resin, alkyd resin, acrylic resin, epoxy modified silicone resin, phenolic resin or vinylite, when resin is solid-state, need before use to smash into solid resin to pieces powder；Described solvent is dehydrated alcohol, dimethylbenzene, n-butyl alcohol, Ketohexamethylene, methyl iso-butyl ketone (MIBK) one or more mixing therein.
10. the preparation method of a kind of Graphene modified anti-corrosive coating as according to any one of claim 14, it is characterised in that: described dispersing technology is high speed magnetic stirring technique, emulsification pretreatment dispersing technology, high speed homogenization dispersed with stirring technique, ball-milling method dispersing technology or sand milling dispersing technology.
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