CN107384184B - Modified graphene nanosheet heavy-duty anticorrosive coating and preparation method thereof - Google Patents
Modified graphene nanosheet heavy-duty anticorrosive coating and preparation method thereof Download PDFInfo
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- CN107384184B CN107384184B CN201710707581.6A CN201710707581A CN107384184B CN 107384184 B CN107384184 B CN 107384184B CN 201710707581 A CN201710707581 A CN 201710707581A CN 107384184 B CN107384184 B CN 107384184B
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The invention discloses a modified graphene nanosheet heavy-duty anticorrosive coating and a preparation method thereof, wherein the coating comprises the following components: acrylic polyurethane resin, graphene nanosheets, a modifier, indene and a drier. Wherein the mass ratio of the components is acrylic polyurethane resin: graphene nanoplatelets: modifying agent: indene oxide: drier = 100: 1-5: 2-10: 30-50: 0.1 to 0.3. According to the heavy-duty anticorrosive coating, the modified graphene nanosheets are combined with the hydroxyl groups in the acrylic polyurethane resin, so that the oxygen-containing functional groups in the system are increased, the crosslinking degree of the coating is improved, and the impedance value of the coating can reach 107~109Omega, has good electrochemical corrosion resistance.
Description
Technical Field
The invention relates to an anticorrosive coating, and in particular relates to a modified graphene nanosheet heavy-duty anticorrosive coating and a preparation method thereof.
Background
The marine corrosion is a common problem in the world at present, and the marine engineering facilities in China are invaded at an incredible speed, so that the safety of the marine engineering facilities is threatened all the time, and the pace of marine economic development in China is greatly hindered. Among all the anti-corrosion measures, the protection by organic coatings, i.e. anti-corrosion coatings, is the most widely, economically and conveniently applied method. The heavy-duty anticorrosive coating is an anticorrosive coating which can be applied in a relatively severe corrosive environment compared with a conventional anticorrosive coating and has a longer protection period than the conventional anticorrosive coating.
The acrylic polyurethane system has the advantages of fast drying, convenient construction, easy construction recoating and reworking and wide application due to the good performances of flexibility, adhesive force, light and color retention, water and chemical resistance, high solid components and the like. However, since the shielding effect and the corrosion resistance are not outstanding, the corrosion resistance of the resin body is often enhanced by adding an additive. The graphene nanosheet is formed by stacking single-layer carbon atom planar structure graphene, is more than 20 times cheaper than graphene, is simple to prepare, is not easy to agglomerate, can play a good shielding role, and has general compatibility with resin.
Through the search of the prior art, Chinese patent with publication number CN105802441A discloses a water-based graphene composite coating, a water-based graphene composite coating and a preparation method thereof, wherein the coating is composed of water-based resin, graphene, aniline oligomer derivatives, water and a coating auxiliary agent, and pi-pi bonds are formed by the graphene and the aniline oligomer derivatives to realize uniform dispersion in the water. The coating has good water permeability resistance and salt fog resistance, but the impedance value of the coating can only reach 105Ω。
The Chinese patent with publication number CN105419437A discloses a graphene modified matched anticorrosive coating and preparation and application thereof, the coating consists of a primer, an intermediate paint and a finish paint, wherein the primer and the intermediate paint are modified graphene coatings, the finish paint is a polyurethane finish paint or a fluorocarbon finish paint, and the modified graphene coating is prepared by mixing a surfactant serving as a modifier with graphene for modification, then uniformly dispersing the mixture in an organic solvent, and then adding the mixture into organic resin, a curing agent and an auxiliary agent. The coating has excellent waterproof permeability and salt spray resistance, but the impedance value can only reach 104Ω。
Chinese patent publication No. CN104946114A discloses a graphene-containing metal surface anticorrosive coating and a preparation method thereof, the coating is formed by drying self-repairing microcapsules uniformly dispersed in a film-forming matrix, wherein the self-repairing microcapsules are formed by coating graphene with an organic repairing agent, and the film-forming matrix comprises an aqueous organic resin, wherein the graphene is selected from graphene oxide, partially reduced graphene oxide, and chemically surface-modified graphene. The invention only shows that the anticorrosive coating can be automatically repaired under the condition of scratching, but the anticorrosive performance of the anticorrosive coating is not tested.
Chinese patent with publication number CN104231703A discloses a graphene composite anticorrosive coatingThe preparation method comprises the steps of forming an organic coating film on the surface of metal by electrodepositing an organic polymer with a plurality of hydroxyl groups or amino groups, forming a film by using a graphene oxide or modified graphene solution, and finally forming a layer of organic coating film on the surface of the metal. The film layer obtained by the method is controllable, compact and uniform, but the operation is more complicated, three times of electrodeposition film forming processes are required, and the impedance value of the composite coating is 105~106Omega is between.
The coatings in the prior art have some defects, such as high cost of graphene and poor compatibility with resin, and the coatings can not meet the performance requirements of heavy-duty anticorrosive coatings and have poor impedance performance.
Disclosure of Invention
The invention aims to provide a modified graphene nanosheet heavy-duty anticorrosive coating and a preparation method thereof, the coating solves the problems of high manufacturing cost and poor corrosion resistance in the prior art, and the impedance value of the coating can reach 107~109Omega, and the crosslinking degree of the coating is high, thereby meeting the performance requirement of the heavy anti-corrosion coating.
In order to achieve the above object, the present invention provides a modified graphene nanoplatelets heavy-duty coating, which comprises the following components: acrylic polyurethane resin, graphene nanosheets, a modifier, indene and a drier.
Wherein the mass ratio of the components is that acrylic polyurethane resin: graphene nanoplatelets: modifying agent: indene oxide: drier = 100: 1-5: 2-10: 30-50: 0.1 to 0.3.
The thickness of the graphene nanosheet is 3-10 nm.
The diameter of the graphene nanosheet is 5-50 microns.
The modifier is sodium dodecyl benzene sulfonate.
The drier comprises: dibutyltin dilaurate or/and N, N-dimethylethanolamine.
The invention also provides a preparation method of the modified graphene nanosheet heavy duty coating, and the method comprises the following steps:
dissolving graphene nanosheets and sodium dodecyl benzene sulfonate in water, adjusting the concentration of the graphene nanosheets to be 0.01g/m L-0.03 g/m L, performing ultrasonic treatment to uniformly disperse the graphene nanosheets, performing suction filtration, washing with ethanol and water in sequence, and drying to obtain modified graphene nanosheets;
step 2: and ultrasonically treating the modified graphene nanosheet in a solvent, then adding the modified graphene nanosheet into acrylic polyurethane resin, sequentially adding the indene oxide and the drier, uniformly mixing, coating the mixture on the surface-treated metal surface, and naturally drying to finish the preparation of the composite coating.
In step 1, the mass of the sodium dodecyl benzene sulfonate is as follows: mass =2 of graphene nanoplatelets: 1.
in step 1, the water is pure water or ultrapure water.
In step 2, the solvent is selected from one or more of ethanol, acetone, toluene, xylene and N-methylpyrrolidone.
In the step 2, the mass of the modified graphene nano sheet to the volume of the solvent is =0.1 g-0.5 g: 1 m L-5 m L.
The modified graphene nanosheet heavy-duty anticorrosive coating and the preparation method thereof solve the problems that the manufacturing cost is high and the performance requirement of the heavy-duty anticorrosive coating cannot be met in the prior art, and have the following advantages:
(1) according to the heavy-duty anticorrosive coating, the modified graphene nanosheets in the heavy-duty anticorrosive coating are combined with the hydroxyl groups in the acrylic polyurethane resin, so that the oxygen-containing functional groups in the system are increased, the crosslinking degree of the coating is improved, and the obtained coating is good in compactness;
(2) the impedance value of the heavy anti-corrosion coating can reach 107~109Omega, which has good resistance to electrochemical corrosion.
Drawings
FIG. 1 is a Fourier transform infrared spectrum of the coatings and blank controls of examples 1-3 of the present invention.
FIG. 2 is a graph of the electrochemical impedance results of the coating of example 1 of the present invention.
FIG. 3 is a graph of the electrochemical impedance results of the coating of example 2 of the present invention.
FIG. 4 is a graph of the electrochemical impedance results of the coating of example 3 of the present invention.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples.
The invention discloses a modified graphene nanosheet heavy-duty anticorrosive coating, which comprises the following components: acrylic polyurethane resin, graphene nanosheets, a modifier, indene and a drier. The mass ratio of the components is acrylic polyurethane resin: graphene nanoplatelets: modifying agent: indene oxide: drier = 100: 1-5: 2-10: 30-50: 0.1 to 0.3. The modified graphene nanosheets are combined with hydroxyl groups in the acrylic polyurethane resin, so that oxygen-containing functional groups in a system are increased, the crosslinking degree of the coating is improved, and the obtained coating is good in compactness. The indene is used as an anticorrosive additive and can prevent the corrosion of the coating. The drier can accelerate the drying of the coating to form a film.
The graphene nanosheet is 3-10 nm in thickness and 5-50 μm in diameter.
The modifier is sodium dodecyl benzene sulfonate which modifies the graphene nanosheet through a non-covalent bond.
The drier comprises: dibutyltin dilaurate or/and N, N-dimethylethanolamine.
The invention discloses a preparation method of a modified graphene nanosheet heavy-duty anticorrosive coating, which comprises the following steps:
dissolving graphene nanosheets and sodium dodecyl benzene sulfonate in water, adjusting the concentration of the graphene nanosheets to be 0.01g/m L-0.03 g/m L, performing ultrasonic treatment to uniformly disperse the graphene nanosheets, reacting the graphene nanosheets with the sodium dodecyl benzene sulfonate to form a pi-pi conjugated non-covalent bond combination form, performing suction filtration, washing with ethanol and water in sequence, and drying to obtain modified graphene nanosheets;
step 2: and ultrasonically treating the modified graphene nanosheet in a solvent, then adding the modified graphene nanosheet into acrylic polyurethane resin, sequentially adding the indene oxide and the drier, uniformly mixing, coating the metal surface treated according to the national standard GB/T18839.2-2002, and naturally drying to finish the preparation of the composite coating.
In step 1, the mass of the sodium dodecyl benzene sulfonate is as follows: mass =2 of graphene nanoplatelets: 1, water is pure water or ultrapure water; the ultrasonic time is 12-18 h; the drying temperature is 70-100 deg.C, under which the excessive sodium dodecylbenzene sulfonate and water are removed.
In the step 2, the solvent is selected from one or more of ethanol, acetone, toluene, xylene and N-methylpyrrolidone, and the mass of the modified graphene nanosheet is that the volume of the solvent is =0.1 g-0.5 g: 1 m L-5 m L.
Example 1
Step 1, weighing 0.1g of graphene nanosheet, carrying out ultrasonic treatment on the graphene nanosheet and 0.2g of sodium dodecyl benzene sulfonate in 10m L ultrapure water for 12 hours, filtering, and drying at 70 ℃ for 4 hours to obtain a modified graphene nanosheet;
and 2, ultrasonically treating the modified graphene nanosheet in 2m L acetone for 30min, adding the modified graphene nanosheet into 10g of acrylic polyurethane resin, adding 3g of indene, adding 3 drops of dibutyltin dilaurate (drier), uniformly mixing, standing for 30 min-2 h, coating the acetone on the surface-treated metal surface after the acetone is completely volatilized, and naturally drying for 24h to finish the preparation.
Example 2
Step 1, weighing 0.2g of graphene nanosheet, carrying out ultrasonic treatment on the graphene nanosheet and 0.4g of sodium dodecyl benzene sulfonate in 10m L ultrapure water for 12 hours, filtering, washing with ethanol and water, and drying to obtain a modified graphene nanosheet;
and 2, ultrasonically treating the modified graphene nanosheets in 3m L xylene for 30min, adding the modified graphene nanosheets into 10g of acrylic polyurethane resin, adding 3g of indene, adding 4 drops of dibutyltin dilaurate, uniformly mixing, standing, coating the metal surface with the modified graphene nanosheets after the xylene is volatilized, and naturally drying for 48h to finish the preparation.
Example 3
Step 1, weighing 0.3g of graphene nanosheet, carrying out ultrasonic treatment on the graphene nanosheet and 0.6g of sodium dodecyl benzene sulfonate in 10m L ultrapure water for 12 hours, filtering, washing with ethanol and water, and drying to obtain a modified graphene nanosheet;
and 2, ultrasonically treating the modified graphene nanosheets in 5m L ethanol for 30min, adding the modified graphene nanosheets into 10g of acrylic polyurethane resin, adding 3g of indene, adding 5 drops of dibutyltin dilaurate, uniformly mixing, standing, coating the metal surface with the modified graphene nanosheets after the ethanol is completely volatilized, and naturally drying for 48h to finish the preparation.
The coatings of examples 1-3 were examined by infrared spectroscopy, and the blank control was an acrylic urethane resin without added graphene nanoplatelets, as shown in fig. 1, which is a fourier transform infrared spectrum of the coatings of examples 1-3 of the present invention and the blank control, and the coatings prepared in example 1 were measured at 1240cm-1The increase of the adjacent C-O bond indicates that the oxygen-containing functional groups in the system are increased, and the crosslinking degree of the modified graphene nano sheet is improved mainly due to the combination of the modified graphene nano sheet and the hydroxyl in the acrylic polyurethane resin; example 2 and example 3 both showed a new peak position of 3190 cm compared to example 1-1And 3050 cm-1And the nearby peak is an N-H stretching vibration peak, which shows that N-H bonds are generated after the graphene nanosheets and isocyanate in the acrylic polyurethane resin are subjected to redox reaction.
The coatings of examples 1 to 3 were subjected to electrochemical impedance tests, and the coatings of examples 1 to 3 were immersed in 3.5% by mass of NaCl solution, respectively, to test the electrochemical impedance properties of the coatings immersed for 1d (day), 7 d, 14 d, 21 d and 28 d. No bubble or rust was observed in examples 1 to 3 during immersion. As shown in FIG. 2, which is a graph showing the electrochemical impedance results of the coating layer of example 1 of the present invention (the abscissa represents the real part of the impedance, and the ordinate represents the imaginary part of the impedance), the coating layer prepared in example 1 can have an impedance value of up to 107Omega; as shown in FIG. 3, which is a graph showing the electrochemical impedance results of the coating layer of example 2 of the present invention (the abscissa represents the real part of the impedance, and the ordinate represents the imaginary part of the impedance), the coating layer prepared in example 2 can have an impedance value of up to 109Omega; FIG. 4 is a graph showing the electrochemical impedance results of the coating of example 3 of the present invention (the abscissa represents the real part of the impedance and the ordinate represents the imaginary part of the impedance), with the real partThe coating prepared in example 3 has a resistance value of up to 107Ω。
The salt spray tests of the coatings and the blank control groups of examples 1 to 3 are carried out, and the salt spray tests of 1000h are carried out according to the national standard GB/T10125-.
In summary, according to the modified graphene nanoplatelet heavy-duty anticorrosive coating and the preparation method thereof, the coating increases oxygen-containing functional groups in a system by combining the modified graphene nanoplatelets with hydroxyl groups in acrylic polyurethane resin, so that the crosslinking degree of the coating is improved, the obtained coating has good compactness, and the impedance value of the coating can reach 107~109Omega, has good electrochemical corrosion resistance.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (8)
1. The modified graphene nanosheet heavy-duty anticorrosive coating is characterized by comprising the following components: acrylic polyurethane resin containing hydroxyl, graphene nanosheets, a modifier, indene and a drier;
the mass ratio of the components is that acrylic polyurethane resin containing hydroxyl: graphene nanoplatelets: modifying agent: indene oxide: drier = 100: 2: 4: 30-50: 0.1 to 0.3;
the modifier is sodium dodecyl benzene sulfonate;
the heavy-duty anticorrosive coating is prepared by the following method:
dissolving graphene nanosheets and sodium dodecyl benzene sulfonate in water, adjusting the concentration of the graphene nanosheets to be 0.01g/m L-0.03 g/m L, performing ultrasonic treatment to uniformly disperse the graphene nanosheets, performing suction filtration, washing with ethanol and water in sequence, and drying to obtain modified graphene nanosheets;
step 2: and ultrasonically treating the modified graphene nanosheet in a solvent, then adding the modified graphene nanosheet into hydroxyl-containing acrylic polyurethane resin, sequentially adding the indene and the drier, uniformly mixing, coating the mixture on the surface of the metal subjected to surface treatment, and naturally drying to finish the preparation of the composite coating.
2. The modified graphene nanosheet heavy duty coating of claim 1, wherein the graphene nanosheet has a thickness of 3-10 nm.
3. The modified graphene nanosheet heavy duty coating of claim 2, wherein the graphene nanosheet has a diameter of 5 μm to 50 μm.
4. The modified graphene nanoplatelet heavy duty coating of claim 1 wherein the drier comprises: dibutyltin dilaurate or/and N, N-dimethylethanolamine.
5. A method for preparing the modified graphene nanoplatelet heavy duty coating according to any one of claims 1 to 4, comprising:
dissolving graphene nanosheets and sodium dodecyl benzene sulfonate in water, adjusting the concentration of the graphene nanosheets to be 0.01g/m L-0.03 g/m L, performing ultrasonic treatment to uniformly disperse the graphene nanosheets, performing suction filtration, washing with ethanol and water in sequence, and drying to obtain modified graphene nanosheets;
step 2: and ultrasonically treating the modified graphene nanosheet in a solvent, then adding the modified graphene nanosheet into hydroxyl-containing acrylic polyurethane resin, sequentially adding the indene and the drier, uniformly mixing, coating the mixture on the surface of the metal subjected to surface treatment, and naturally drying to finish the preparation of the composite coating.
6. The preparation method of the modified graphene nanoplatelet heavy-duty coating according to claim 5, wherein in step 1, the mass of the sodium dodecylbenzenesulfonate is as follows: mass =2 of graphene nanoplatelets: 1.
7. the method for preparing the modified graphene nanoplatelet heavy-duty coating according to claim 5, wherein in step 1, the water is ultrapure water.
8. The method for preparing the modified graphene nanoplatelets heavy anti-corrosion coating according to claim 5, wherein in the step 2, the solvent is selected from any one or more than two of ethanol, acetone, toluene, xylene and N-methylpyrrolidone.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105419437A (en) * | 2015-12-24 | 2016-03-23 | 中国科学院海洋研究所 | Supporting anti-corrosive coating modified by graphene, preparation and application thereof |
| CN106867298A (en) * | 2017-03-15 | 2017-06-20 | 中国科学院宁波材料技术与工程研究所 | The preparation method of graphite alkenes anticorrosive paint |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105419437A (en) * | 2015-12-24 | 2016-03-23 | 中国科学院海洋研究所 | Supporting anti-corrosive coating modified by graphene, preparation and application thereof |
| CN106867298A (en) * | 2017-03-15 | 2017-06-20 | 中国科学院宁波材料技术与工程研究所 | The preparation method of graphite alkenes anticorrosive paint |
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