CN110746853A - Preparation method of hydroxylated graphene powder coating - Google Patents
Preparation method of hydroxylated graphene powder coating Download PDFInfo
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- CN110746853A CN110746853A CN201911059186.7A CN201911059186A CN110746853A CN 110746853 A CN110746853 A CN 110746853A CN 201911059186 A CN201911059186 A CN 201911059186A CN 110746853 A CN110746853 A CN 110746853A
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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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/06—Polyethene
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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
- C09D133/04—Homopolymers or copolymers of esters
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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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
- C09D5/038—Anticorrosion agents
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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
-
- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
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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)
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Abstract
The invention discloses a preparation method of a hydroxylated graphene powder coating, which comprises the following components in parts by weight: 0.5-5 parts of hydroxylated graphene, 70-90 parts of powder coating, 1-3 parts of pigment, 3-5 parts of powder leveling agent, ethanol or deionized water and other solvents. The preparation method comprises the steps of carrying out ball milling dispersion on the hydroxylated graphene, the powder coating and the powder type flatting agent in a horizontal ball mill, removing the solvent, and then carrying out film coating forming through a fluidized bed. The hydroxylated graphene powder anticorrosive paint is safe, environment-friendly, stable in storage, excellent in adhesive force on substrates such as steel and iron, excellent in mechanical properties such as flexibility and wear resistance and the like; the protective effect is outstanding in chemical media such as acid, alkali, salt and the like; the coating has excellent high and low temperature resistance, high salinity resistance and other protective properties under simulated marine environment experimental conditions, and can be applied to priming paint of various steel and iron material marine engineering anticorrosive coatings.
Description
Technical Field
The invention relates to a powder anticorrosive paint, and particularly relates to a preparation method of a hydroxylated graphene powder anticorrosive paint.
Background
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like. The powder coating has the characteristics of no solvent pollution, 100 percent film forming and low energy consumption. However, the powder coating has poor adhesion to metal and poor corrosion resistance, and a proper amount of filler is required to be added for improvement.
Graphene is a carbon atom sp2The hexagonal honeycomb lattice planar thin film composed of the hybrid tracks is a two-dimensional material with the thickness of only one carbon atom, is also the thinnest and hardest nano material known in the world so far, and has the characteristics of ultrahigh specific surface area, excellent conductivity, ultrahigh strength, toughness, shielding property and the like, so that the hexagonal honeycomb lattice planar thin film is expected to play an excellent role in the fields of conductive coatings and metal anticorrosive coatings. However, graphene is a loose nano material, has a large surface energy, and is very easy to agglomerate in a coating matrix, which limits the application of graphene in the coating.
At present, the dispersion stability of graphene in a coating matrix is basically improved through the optimization of a dispersion process and the chemical modification treatment of the surface of the graphene; although the cost of the former is relatively low, the method adds additional steps on the basis of the preparation process of the coating, greatly increases the cost and is not beneficial to industrialization. According to the invention, the graphene is subjected to hydroxylation treatment on the surface, so that the hydrophilic property of the graphene is enhanced, and the agglomeration capability of the graphene in a coating matrix is reduced, thereby improving the dispersibility in the coating matrix and enhancing the comprehensive performance of the powder coating.
Disclosure of Invention
In order to further enhance the acid and alkali resistance, the corrosion resistance, the mechanical strength, the metal adhesion and other properties of the anticorrosive powder coating, the invention provides a method for modifying the powder coating by using hydroxylated graphene.
In order to achieve the purpose, the invention provides the following technical scheme, and the specific manufacturing steps are as follows:
(1) stirring a proper amount of graphene powder in hydrogen peroxide, vanadium pentoxide and a water solution with the pH of 3-5, carrying out ultrasonic treatment and the like to obtain a hydroxylated graphene solution, washing, filtering, freezing and drying to obtain hydroxylated graphene powder;
(2) stirring and dispersing hydroxylated graphene in ethanol or deionized water to prepare 1g/L hydroxylated graphene solution;
(3) stirring and mixing 70-90 parts of powder coating, 1-3 parts of pigment, 3-5 parts of powder type leveling agent and 0.5-5 parts of hydroxylated graphene solution, and placing the mixture in a horizontal ball mill for ball milling for 48-96 hours;
(4) transferring the ball-milled mixture to a beaker and removing the solvent in an oven;
(5) the solvent-removed material was subjected to fluidized bed treatment and the samples were coated on tinplate and tested for corrosion resistance by the salt spray test.
Preferably, the method comprises the following steps: the powder coating is one or more of epoxy powder coating, acrylate powder coating, polyethylene powder coating and fluororesin powder coating.
Preferably, the method comprises the following steps: the addition amount of the hydroxylated graphene is one of 0.5-1 part, 1-3 parts and 3-5 parts.
The hydroxylated graphene powder anticorrosive paint is safe, environment-friendly, stable in storage, excellent in adhesive force on substrates such as steel and iron, excellent in mechanical properties such as flexibility and wear resistance and the like; the protective effect is outstanding in chemical media such as acid, alkali, salt and the like; the coating has excellent high and low temperature resistance, high salinity resistance and other protective properties under simulated marine environment experimental conditions, and can be applied to priming paint of various steel and iron material marine engineering anticorrosive coatings.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1
A method for modifying powder coating by hydroxylated graphene comprises the following specific operation steps:
(1) stirring a proper amount of graphene powder in hydrogen peroxide, vanadium pentoxide and a water solution with the pH of 3-5, carrying out ultrasonic treatment and the like to obtain a hydroxylated graphene solution, washing, filtering, freezing and drying to obtain hydroxylated graphene powder;
(2) stirring and dispersing hydroxylated graphene in ethanol or deionized water to prepare 1g/L hydroxylated graphene solution;
(3) stirring and mixing 60-90 parts of epoxy powder coating, 1-3 parts of pigment, 3-5 parts of powder type flatting agent and 1-3 parts of hydroxylated graphene solution, and placing the mixture in a horizontal ball mill for ball milling for 48-96 hours;
(4) transferring the ball-milled mixture to a beaker and removing the solvent in an oven;
(5) stirring and mixing the mixture of which the solvent is removed in the step (4) and an anhydride epoxy resin curing agent;
(6) and (3) treating the substance in the step (5) by a fluidized bed, coating a sample on a tinplate, and testing the corrosion resistance of the tinplate by a salt spray test.
Example 2
A method for modifying powder coating by hydroxylated graphene comprises the following specific operation steps:
(1) stirring a proper amount of graphene powder in hydrogen peroxide, vanadium pentoxide and a water solution with the pH of 3-5, carrying out ultrasonic treatment and the like to obtain a hydroxylated graphene solution, washing, filtering, freezing and drying to obtain hydroxylated graphene powder;
(2) stirring and dispersing hydroxylated graphene in ethanol or deionized water to prepare 1g/L hydroxylated graphene solution;
(3) stirring and mixing 70-90 parts of polyethylene powder coating, 1-3 parts of pigment, 3-5 parts of powder type leveling agent and 1-3 parts of hydroxylated graphene solution, and placing the mixture in a horizontal ball mill for ball milling for 48-96 hours;
(4) transferring the ball-milled mixture to a beaker and removing the solvent in an oven;
(5) and (4) treating the substance in the step (4) by a fluidized bed, coating a sample on a tinplate, and testing the corrosion resistance of the tinplate by a salt spray test.
Example 3
A method for modifying powder coating by hydroxylated graphene comprises the following specific operation steps:
(1) stirring a proper amount of graphene powder in hydrogen peroxide, vanadium pentoxide and a water solution with the pH of 3-5, carrying out ultrasonic treatment and the like to obtain a hydroxylated graphene solution, washing, filtering, freezing and drying to obtain hydroxylated graphene powder;
(2) stirring and dispersing hydroxylated graphene in ethanol or deionized water to prepare 1g/L hydroxylated graphene solution;
(3) stirring and mixing 70-90 parts of polytetrafluoroethylene powder, 1-3 parts of pigment, 3-5 parts of powder type flatting agent and 1-3 parts of hydroxylated graphene solution, and placing the mixture in a horizontal ball mill for ball milling for 48-96 hours;
(4) transferring the ball-milled mixture to a beaker and removing the solvent in an oven;
(5) and (4) treating the substance in the step (4) by a fluidized bed, coating a sample on a tinplate, and testing the corrosion resistance of the tinplate by a salt spray test.
The powder coating sample obtained by modifying the hydroxylated graphene is subjected to experimental comparison tests, and the results are shown in the following table:
| item | Salt spray test for 5% salt solution for 500h | Salt spray test of 5% salt solution for 1000h | Adhesion test (cross cut method) |
| Example 1 | Without obvious change | Without obvious change | 5B |
| Pure epoxy resin coating | Bubbling and falling off | The coating is seriously peeled off | 5B |
| Example 2 | Without obvious change | Without obvious change | 5B |
| Pure polyethylene coating | Bubbling and falling off | Part of the coating is removed | 5B |
| Example 3 | Without obvious change | Without obvious change | 5B |
| Pure polytetrafluoroethylene coating | Without obvious change | Bubbling of part of the coating | 5B |
The data in the table are compared to show that: after a small amount of hydroxylated graphene is added, the salt spray resistance of the powder coating is obviously improved, and the adhesive force is not obviously changed.
Claims (3)
1. A preparation method of a hydroxylated graphene powder coating is characterized by comprising the following specific experimental steps:
(1) stirring a proper amount of graphene powder in hydrogen peroxide, vanadium pentoxide and a water solution with the pH of 3-5, carrying out ultrasonic treatment and the like to obtain a hydroxylated graphene solution, washing, filtering, freezing and drying to obtain hydroxylated graphene powder;
(2) dispersing hydroxylated graphene and a powder coating;
(3) and (5) film forming and corrosion resistance testing.
2. The preparation method according to claim 1, wherein the dispersing of the hydroxylated graphene and the powder coating in the step (2) comprises the following specific steps:
(1) stirring and dispersing hydroxylated graphene in ethanol or deionized water to prepare 1g/L hydroxylated graphene solution;
(2) stirring and mixing the powder coating, the pigment, the powder leveling agent and the hydroxylated graphene solution, and placing the mixture in a horizontal ball mill for ball milling for 48-96 hours;
(3) the ball milled mixture was transferred to a beaker and the solvent was removed in an oven.
3. The preparation method according to claim 1, wherein the coating film in the step (3) is formed, and the corrosion resistance test specifically comprises the following steps: the solvent-removed mixture was subjected to a fluidized bed treatment and the sample was coated on tinplate and tested for corrosion resistance by the salt spray test.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911059186.7A CN110746853A (en) | 2019-11-01 | 2019-11-01 | Preparation method of hydroxylated graphene powder coating |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911059186.7A CN110746853A (en) | 2019-11-01 | 2019-11-01 | Preparation method of hydroxylated graphene powder coating |
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| CN110746853A true CN110746853A (en) | 2020-02-04 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371537A (en) * | 2014-10-20 | 2015-02-25 | 航天科工防御技术研究试验中心 | Anticorrosive paint and preparation method thereof |
| CN107665982A (en) * | 2017-08-04 | 2018-02-06 | 郴州国盛新材科技有限公司 | A kind of vanadic anhydride/graphene composite material and preparation method thereof |
| CN108281216A (en) * | 2017-12-25 | 2018-07-13 | 常州二维碳素科技股份有限公司 | A kind of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry and its preparation method and application |
| CN109456681A (en) * | 2018-10-26 | 2019-03-12 | 四川大学 | A kind of preparation method of the graphene of anti-corrosive properties/powder thermosetting composite coating |
| CN110373070A (en) * | 2019-06-13 | 2019-10-25 | 深圳诺必达节能环保有限公司 | A kind of high-intensitive heating anti-corrosion Graphene powder powder material and its preparation method and application |
-
2019
- 2019-11-01 CN CN201911059186.7A patent/CN110746853A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371537A (en) * | 2014-10-20 | 2015-02-25 | 航天科工防御技术研究试验中心 | Anticorrosive paint and preparation method thereof |
| CN107665982A (en) * | 2017-08-04 | 2018-02-06 | 郴州国盛新材科技有限公司 | A kind of vanadic anhydride/graphene composite material and preparation method thereof |
| CN108281216A (en) * | 2017-12-25 | 2018-07-13 | 常州二维碳素科技股份有限公司 | A kind of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry and its preparation method and application |
| CN109456681A (en) * | 2018-10-26 | 2019-03-12 | 四川大学 | A kind of preparation method of the graphene of anti-corrosive properties/powder thermosetting composite coating |
| CN110373070A (en) * | 2019-06-13 | 2019-10-25 | 深圳诺必达节能环保有限公司 | A kind of high-intensitive heating anti-corrosion Graphene powder powder material and its preparation method and application |
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