CN108424705B - A kind of high dispersion modified graphene oxide, preparation method and its anticorrosive paint - Google Patents
A kind of high dispersion modified graphene oxide, preparation method and its anticorrosive paint Download PDFInfo
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- CN108424705B CN108424705B CN201810214204.3A CN201810214204A CN108424705B CN 108424705 B CN108424705 B CN 108424705B CN 201810214204 A CN201810214204 A CN 201810214204A CN 108424705 B CN108424705 B CN 108424705B
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- graphene oxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—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 a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
- 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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- 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
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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
- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of high dispersion modified graphene oxide, preparation method and its anticorrosive paints, and graphene oxide and 3- aminobenzene acid reaction are obtained the boric acid modified graphene oxide of 3- aminobenzene；Isocyanuric acid three-glycidyl ester and the boric acid modified graphite oxide alkene reaction of 3- aminobenzene are obtained into high dispersion modified graphene oxide, stability is good, dispersed height；The high dispersion modified graphene oxide is uniformly dispersed with matrix resin, levelling agent, defoaming agent, dispersing agent, coalescing agent, diluent further, obtains anticorrosive paint, antiseptic property is good, long service life.Present invention process is simple, environment-friendly high-efficiency, is suitable for industrialized production.
Description
Technical field
The invention belongs to the technical field of coating preparation, a kind of high dispersion modified graphene oxide, its preparation side are provided
Method and its anticorrosive paint.
Background technique
Corrosion protection plays outstanding role in contemporary metal processing industry.Mass data indicate, corrosion to national economy with
And industrialization development causes heavy losses.Wherein marine ship corrosion accounts for very big one side, and marine corrosion causes very hull
Big waste, and become potential security risk.Graphene causes as a kind of New Two Dimensional material, excellent physicochemical property
Extensive concern.The performances such as the bigger serface of graphene, excellent electricity, optics enable it all present in every field tempting
Prospect, when graphene is applied in anticorrosive paint, graphene have the function of physical isolation and electronics conduction.Graphene
The conjugated structure of lamella is layering to form fine and close isolation layer in the coating, obstructs infiltration and infiltration of the moisture to film
Thoroughly --- play physical preservation, graphene surface hydrophobic property strengthens moisture penetration.
Application No. is 201610878263.1 Chinese patent applications to make stone by carrying out secondary oxidation modification to graphene
The stability of black alkene increases, and is conducive to the corrosion resistance for utmostly playing graphene itself, has the coating prepared
Excellent adhesive force, hardness, wearability and resistance to Neutral Salt Spray Corrosion, but this method material requested is more, and preparation process is complicated,
Higher cost, and dispersibility and resistance to acid and alkali are bad.
The mode majority that graphene is applied to coating at present is added graphene as functional filler, thus band
Come a critical issue is how to solve the dispersion stabilization problem of graphene, needs to be modified graphene.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of high dispersion modified graphene oxide, its preparation are provided
Method and its anticorrosive paint.
The technical solution adopted by the present invention to solve the technical problems first is that:
A kind of preparation method of high dispersion modified graphene oxide, includes the following steps:
1) by graphene oxide and 3- amino phenyl boric acid with the quality of 1~10:1 than ultrasonic disperse in the first solvent, rise
Temperature is separated by solid-liquid separation to 60~120 DEG C of 4~10h of back flow reaction, obtains the boric acid modified graphene oxide of 3- aminobenzene；
2) the boric acid modified graphene oxide of 3- aminobenzene for obtaining isocyanuric acid three-glycidyl ester and step 1) with 1~
The quality of 15:1 in the second solvent, is warming up to 80~180 DEG C of back flow reactions 12~for 24 hours than ultrasonic disperse, is separated by solid-liquid separation, obtains
The modified graphene oxide.
In a preferred embodiment of the invention, first solvent is at least one of water, toluene.
In a preferred embodiment of the invention, second solvent is n,N-Dimethylformamide, N- methyl pyrrole
At least one of pyrrolidone.
The technical solution adopted by the present invention to solve the technical problems second is that:
A kind of graphene oxide high dispersion modified according to prepared by above-mentioned preparation method.
The technical solution adopted by the present invention to solve the technical problems third is that:
A kind of anticorrosive paint includes following component according to the mass fraction:
Described matrix resin is epoxy resin, fluorocarbon resin, amino resins, acrylic resin, polyurethane resin, alkyd tree
At least one of rouge, polyester resin.
The levelling agent is at least one of organosilicon, acrylic compounds, only son's ethers.
The defoaming agent be at least one of organic silicon defoaming agent, inorganic silicon class defoaming agent, antifoaming agent of non-silicone,
As BYK302, BYK065 of German Bi Ke company production, BYK20, BYK011, BYK053, Efka company produce
At least one of Efka2018.
The dispersing agent is at least one of self-fluxing nature dispersing agent, wetting dispersing agent, as Bi Ke company, Germany produces
At least one of BYK101, BYK161, BYK163, Efka5044 of Efka company production.
The coalescing agent is butyl Bian alcohol acetic ester, butyl glycol ether alkyd rouge, ethylene glycol phenyl ether, dibasic acid dimethyl ester
At least one of class, propylene glycol propyl ether, binary acids diethyl esters class.
The diluent is 1,4- butanediol diglycidyl ether, ethylene glycol diglycidylether, acetone, dimethylbenzene, just
At least one of butanol, methyl iso-butyl ketone (MIBK), dehydrated alcohol, ethyl acetate, butyl acetate.
The technical solution adopted by the present invention to solve the technical problems fourth is that:
The preparation method of the anticorrosive paint:
The method comprises the steps of firstly, preparing a kind of high dispersion modified graphene oxides, take 0.5~2 part by anticorrosive paint component proportion
Modified graphene oxide, 40~80 parts of matrix resins, 0.2~1.0 part of levelling agent, 0.05~1.0 part of defoaming agent, 0.1~1.0 part
Dispersing agent, 0.2~1.0 part of coalescing agent, 5~35 parts of diluents.2000~5000r/min of revolving speed is used in high speed disperser
Anticorrosive paint can be obtained after filtering in evenly dispersed 2~6h.
High dispersion modified graphene oxide anti-corrosive aids preparation principle in the present invention: graphene oxide progress surface is changed
Property, 3- amino phenyl boric acid is incorporated in surface of graphene oxide by way of covalent bond, and then modify isocyanuric acid three shrink it is sweet
Grease enhances it with matrix resin compatibility.
The beneficial effects of the present invention are:
1. operating procedure of the invention is simple, environment-friendly high-efficiency, it is suitable for industrialized production.
2. the present invention is directly prepared for high dispersion modified graphene oxide as anti-corrosive aids, phenyl boric acid has rust inhibition
Can, graphene has antiseptic property, can utilize inhibition and the antiseptic property of phenyl boric acid and graphene simultaneously, play composite anti-corrosive
Effect.Isocyanuric acid three-glycidyl ester makes graphene and matrix resin have good compatibility simultaneously, and can participate in resin
Co-curing process.
3. high dispersion modified graphene oxide provided by the invention, stability is good, dispersed height, can be by simply mixed
Modified graphene is added in finished product coating by conjunction process, very convenient.
4. high dispersion modified graphene oxide anti-corrosive aids provided by the invention dispersibility enhancing in coating, graphene
Good dispersion makes its interface binding power with coating matrix with regard to stronger, and the antiseptic property of coating is with regard to more preferable, and coating weatherability
More preferably, the service life is longer.
Detailed description of the invention
Fig. 1 is high dispersion modified graphene oxide preparation process schematic diagram in the present invention.
Fig. 2 is the optical photograph figure of high dispersion modified graphite oxide anti-corrosive aids dispersion liquid made from the embodiment of the present invention 1.
Left figure is the common graphene oxide dispersion placed one week, can generate many precipitatings, and right figure is that the placement one week present invention is real
High dispersion modified graphene oxide made from example 1 is applied, it is still well dispersed.
Fig. 3 is the scanning electron microscope of high dispersion modified graphene oxide anti-corrosive aids made from the embodiment of the present invention 1
(SEM) figure.
Specific embodiment
The contents of the present invention are illustrated below by embodiment:
Technical solution of the present invention is further explained and described below by way of specific embodiment combination attached drawing.
Embodiment antiseptic property is as shown in table 1
Embodiment 1
(1) high dispersion modified graphene oxide is prepared:
A) it takes 0.2g graphene oxide and 0.2g 3- amino phenyl boric acid ultrasonic disperse in toluene, is warming up to 100 DEG C of reflux
6h is reacted, filters and washs to obtain the boric acid modified graphene oxide of 3- aminobenzene；
B) the boric acid modified graphene oxide 0.1g of the 3- aminobenzene for taking step a) to obtain and 1g isocyanuric acid three-glycidyl
Ester is heated to 150 DEG C of back flow reactions for 24 hours in 100mL n,N-Dimethylformamide, filters and washs to obtain high dispersion modified
Graphene oxide.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared
High dispersion modified graphene oxide, 50g epoxy resin, the 0.5g organosilicon, 0.2g defoaming for taking 1g step (1) to prepare
Agent BYK302,0.5g dispersant B YK101,0.5g ethylene glycol phenyl ether, the mixing of 20g 1,4-butanediol diglycidyl ether, in height
The evenly dispersed 4h of 2000~5000r/min of revolving speed is used on fast dispersion machine, and high dispersion modified graphite oxide can be obtained after filtering
Alkene composite anticorrosion coating.
Embodiment 2
(1) high dispersion modified graphene oxide is prepared；
With embodiment 1.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared；
It is 0.5g by the Mass adjust- ment of graphene oxide high dispersion modified in embodiment 1.
Embodiment 3
(1) high dispersion modified graphene oxide is prepared；
With embodiment 1.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared；
It is 1.5g by the Mass adjust- ment of graphene oxide high dispersion modified in embodiment 1.
Embodiment 4
(1) high dispersion modified graphene oxide is prepared；
With embodiment 1.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared；
It is 80g by the Mass adjust- ment of epoxy resin in embodiment 1.
Embodiment 5
(1) high dispersion modified graphene oxide is prepared；
A) 2g graphene oxide and 0.2g 3- amino phenyl boric acid ultrasonic disperse Yu Shuizhong are taken, 120 DEG C of back flow reactions are warming up to
4h is filtered and is washed to obtain the boric acid modified graphene oxide of 3- aminobenzene；
B) the boric acid modified graphene oxide 0.1g and 0.1g isocyanuric acid three of the 3- aminobenzene for taking step a) to obtain shrinks sweet
Grease is heated to 80 DEG C of back flow reaction 18h in 100mL n,N-Dimethylformamide, filters and washs to obtain high dispersion modified
Graphene oxide.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared；
High dispersion modified graphene oxide, the 75g acrylic resin, 0.8g organosilicon, 0.05g for taking 2g step (1) to prepare
Defoaming agent Efka2018,0.9g dispersing agent Efka5044,0.3g butyl Bian alcohol acetic ester, the mixing of 8g acetone, in high speed disperser
It is upper to use the evenly dispersed 6h of 2000~5000r/min of revolving speed, it is compound anti-that high dispersion modified graphene oxide can be obtained after filtering
Rotten coating.
Embodiment 6
(1) high dispersion modified graphene oxide is prepared；
A) it takes 1g graphene oxide and 0.2g 3- amino phenyl boric acid ultrasonic disperse in toluene, it is anti-to be warming up to 60 DEG C of reflux
10h is answered, filter and washs to obtain the boric acid modified graphene oxide of 3- aminobenzene；
B) the boric acid modified graphene oxide 0.1g and 1.5g isocyanuric acid three of the 3- aminobenzene for taking step a) to obtain shrinks sweet
Grease is heated to 180 DEG C of back flow reaction 12h in 100mL N-Methyl pyrrolidone, filters and washs to obtain high dispersion modified
Graphene oxide.
(2) high dispersion modified graphene oxide composite anticorrosion coating is prepared；
High dispersion modified graphene oxide, 45g fluorocarbon resin, 0.3g organosilicon, the 0.9g for taking 0.8g step (1) to prepare disappear
Infusion BYK011,0.05g dispersant B YK163,0.9g propylene glycol propyl ether, the mixing of 30g methyl iso-butyl ketone (MIBK), in high speed disperser
It is upper to use the evenly dispersed 10h of 2000~5000r/min of revolving speed, it is compound anti-that high dispersion modified graphene oxide can be obtained after filtering
Rotten coating.
Examples 1 to 4 antiseptic property test result is as shown in table 1, and GB/T 9274- is pressed in the measurement of floating coat resistance to salt water
88 execute test, and the test of coating salt spray corrosion resistance executes test according to GB/T 1771-2007.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Salt water resistance h | 2520 | 2352 | 2616 | 2256 |
| Salt spray resistance h | 1944 | 1800 | 1992 | 1848 |
The above is only the preferred embodiment of the present invention, the range implemented of the present invention that therefore, it cannot be limited according to, i.e., according to
Equivalent changes and modifications made by the invention patent range and description, should still be within the scope of the present invention.
Claims (10)
1. a kind of preparation method of modified graphene oxide, it is characterised in that: include:
1) by graphene oxide and 3- amino phenyl boric acid with the quality of 1~10:1 than ultrasonic disperse in the first solvent, be warming up to
60~120 DEG C of 4~10h of back flow reaction are separated by solid-liquid separation, obtain the boric acid modified graphene oxide of 3- aminobenzene；
2) the boric acid modified graphene oxide of 3- aminobenzene for obtaining isocyanuric acid three-glycidyl ester and step 1) is with 1~15:1
Quality than ultrasonic disperse in the second solvent, be warming up to 80~180 DEG C of back flow reactions 12~for 24 hours, be separated by solid-liquid separation, obtain described
Modified graphene oxide.
2. preparation method according to claim 1, it is characterised in that: first solvent is water, at least one in toluene
Kind；Second solvent is at least one of N,N-dimethylformamide, N-Methyl pyrrolidone.
3. modified graphene oxide prepared by a kind of preparation method according to claim 1 or 2.
4. a kind of anticorrosive paint, it is characterised in that: according to the mass fraction include following component:
Described matrix resin be epoxy resin, fluorocarbon resin, amino resins, acrylic resin, polyurethane resin, alkyd resin,
At least one of polyester resin.
5. anticorrosive paint according to claim 4, it is characterised in that: the levelling agent is organosilicon, acrylic compounds, only son
At least one of ethers.
6. anticorrosive paint according to claim 4, it is characterised in that: the defoaming agent is organic silicon defoaming agent, non-has
At least one of machine silicon defoaming agent；The dispersing agent is at least one of self-fluxing nature dispersing agent, wetting dispersing agent.
7. anticorrosive paint according to claim 6, it is characterised in that: the antifoaming agent of non-silicone is the defoaming of inorganic silicon class
Agent.
8. anticorrosive paint according to claim 6, it is characterised in that: the defoaming agent be BYK302, BYK065, BYK20,
At least one of BYK011, BYK053, Efka2018；The dispersing agent is BYK101, BYK161, BYK163, Efka5044
At least one of.
9. anticorrosive paint according to claim 4, it is characterised in that: the coalescing agent is butyl Bian alcohol acetic ester, second
Glycol butyl ether alkyd rouge, ethylene glycol phenyl ether, dibasic acid dimethyl ester, propylene glycol propyl ether, at least one in binary acids diethyl esters class
Kind；The diluent be 1,4- butanediol diglycidyl ether, ethylene glycol diglycidylether, acetone, dimethylbenzene, n-butanol,
At least one of methyl iso-butyl ketone (MIBK), dehydrated alcohol, ethyl acetate, butyl acetate.
10. the preparation method of anticorrosive paint described in a kind of any one of claim 4 to 9, it is characterised in that: press the quality
Number takes each component, the evenly dispersed 2~6h of 2000~5000r/min of revolving speed, and filtering obtains the anticorrosive paint.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109749500B (en) * | 2018-12-29 | 2020-05-12 | 厦门大学 | Graphene/azobenzene polymer composite anticorrosive paint additive and preparation method thereof |
| CN110003776B (en) * | 2019-04-28 | 2020-11-20 | 苏州格瑞丰纳米科技有限公司 | Water-based epoxy zinc-rich anticorrosive paint and preparation method and application thereof |
| CN110067001B (en) * | 2019-05-13 | 2020-02-21 | 北京净油洁宝科技有限公司 | Metal cleaning agent and preparation method thereof |
| CN111978771B (en) * | 2019-05-21 | 2022-03-01 | 中车唐山机车车辆有限公司 | Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method |
| CN111019479A (en) * | 2019-12-20 | 2020-04-17 | 佛山科学技术学院 | Coating and preparation method thereof |
| CN112812652B (en) * | 2020-12-31 | 2022-02-25 | 中环涂层技术(广东)有限公司 | Resistance to HCl-H2S corrosion and high temperature resistant coating and preparation method thereof |
| CN115572518A (en) * | 2022-09-26 | 2023-01-06 | 厦门大学 | Water-based concrete protective coating composition and preparation method thereof |
| CN117070126B (en) * | 2023-09-28 | 2024-03-05 | 北京景泰消防科技有限公司 | Corrosion-resistant water-based fireproof paint and preparation method thereof |
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