CN113956696B - Matte graphene coating and preparation method thereof - Google Patents
Matte graphene coating and preparation method thereof Download PDFInfo
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- CN113956696B CN113956696B CN202111306940.XA CN202111306940A CN113956696B CN 113956696 B CN113956696 B CN 113956696B CN 202111306940 A CN202111306940 A CN 202111306940A CN 113956696 B CN113956696 B CN 113956696B
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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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
- C09D7/42—Gloss-reducing 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
- 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
Abstract
The invention discloses a matte graphene coating and a preparation method thereof, wherein the matte graphene coating is composed of 10-35 parts of polyurethane resin, 20-40 parts of graphene resin slurry, 15-30 parts of monomers, 0.2-2 parts of additives, 5-10 parts of photoinitiators and 15-25 parts of matte slurry, wherein the graphene resin slurry is composed of the following raw materials in parts by weight: 30-50 parts of epoxy resin, 1-5 parts of organic bentonite, 35-45 parts of ethanol, 1-15 parts of graphene and 5-10 parts of polyvinylpyrrolidone. The matte graphene coating provided by the invention is simple in preparation method, the prepared graphene epoxy coating has the characteristics of good adhesive force and higher mechanical strength, and the matte coating is soft and good in hand feeling and has outstanding antifouling property.
Description
Technical Field
The invention belongs to the technical field of graphene coatings, and particularly relates to a matte graphene coating and a preparation method thereof.
Background
The high-gloss paint is popular with consumers due to high gloss and gorgeous color, but visual fatigue is easily caused when the high-gloss paint is in the high-gloss environment for a long time, and normal work and life of people are influenced. In addition, the gloss performance requirements of the coating vary due to differences in the objects to be coated and the environment in which they are used. In recent years, people have changed their aesthetic concepts and sensory requirements, and high-grade matte coatings are gaining more and more consumers' favor with their natural and elegant appearance. In addition, the matte coating can shield the defects of a fine paint film on the surface, so that the appearance is uniform and consistent, and compared with a high-gloss coating, the matte coating is simple in construction and has high cost performance. Accordingly, the demand for a gloss coating in the market is also increasing year by year.
It is known that when a light beam is irradiated on a smooth and flat surface, the light beam will be specularly reflected in a reflection angle direction equal to the incident angle, and the light beam has a strong reflection capability, so that a high-gloss surface can be obtained. When light is irradiated on a rough and uneven surface, a diffuse reflection or scattering phenomenon occurs in all directions, thereby obtaining a low-gloss surface. Therefore, the extinction method of the coating mainly changes the originally flat and smooth coating surface into unevenness to form certain roughness, thereby increasing the scattering effect on light and reducing the surface glossiness of the coating.
There are three main ways to reduce the gloss of the coating: one is that inorganic granular matting agent is added, which protrudes the surface of the coating film in the process of solvent volatilization and coating thinning, so that the surface of the coating is uneven to form certain roughness, and the specular reflection of light is weakened; the second one is that polymer with dulling performance is selected as paint film forming matter or added into other paint base body to form some spherical grains on the surface or base body with different shrinkage degree, and the solvent is volatilized to produce molecular curling to result in no smooth surface, change the light reflecting effect and lower the coating brightness. And thirdly, the smooth surface of the formed coating is damaged by methods such as sand blasting, etching, hot working or solvent corrosion, and the like, so that a certain rough surface is obtained, but the cost is further increased due to the increase of the preparation process, and the other properties of the coating are negatively affected due to the solvent corrosion. Thus, the first two approaches are the primary paint matting methods.
However, for graphene coatings, the gloss often needs to be adjusted in the preparation process of finished products, and the extinction powder is usually added directly. However, the way of directly adding the matting powder has some inevitable problems: due to the porous nature and the large structural property of surface energy of fumed silica, sufficient time and shear strength are needed originally for wetting and dispersing, and the viscosity of a material to be a finished product is not as high as that of a material in premixing, so that the wetting and dispersing of the matting powder are increased by prolonging the stirring time and increasing the shear rate, which is a common treatment method, however, manpower and material resources are needed to be added, and the solvent volatilization caused in the process of stirring again possibly influences the final index detection of the finished product, even has negative influence on the application performance. Meanwhile, due to the strong van der waals acting force existing among the graphene, the graphene cannot be stably dispersed in a solvent, and is easy to agglomerate together again after being dispersed, so that the application of the graphene is restricted.
Therefore, there is a need in the art for a graphene coating that is matte, soft to the touch, and good in stain resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a matte graphene coating and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a matte graphene coating is prepared from the following raw materials in parts by weight:
the graphene resin slurry is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 1-5 parts of organic bentonite, 35-45 parts of ethanol, 1-15 parts of graphene and 5-10 parts of polyvinylpyrrolidone.
Preferably, the matte graphene coating is prepared from the following raw materials in parts by weight:
preferably, the matte graphene coating is prepared from the following raw materials in parts by weight:
preferably, the monomer is one or more of acrylic acid and acrylate containing epoxy groups, hydroxyl groups, nitrile groups, carboxylic acid groups, ether groups, amino groups, amide groups, benzene rings, saturated rings, alkoxy groups and silicon atoms.
Preferably, the additive is one or more of simethicone, phenethyl alcohol oleate, organosiloxane, polyether, sodium carboxymethyl cellulose, polyethylene glycol, polyvinyl alcohol and polyethylene wax.
Preferably, the photoinitiator is one or more of phosphazene, phosphorus nitrile salt, phosphonitrile oxide, azobisisobutyronitrile, azobisisovaleronitrile benzil ketal, benzoyl formate, benzophenone and tertiary amine accelerators.
Preferably, the preparation method of the graphene resin slurry comprises the following steps:
uniformly mixing epoxy resin, organic bentonite and ethanol, and then performing infiltration treatment on graphene; and after the infiltration treatment is finished, adding polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and performing ultrasonic dispersion for 30min to obtain the stable graphene resin slurry.
Preferably, the matte slurry is 25-40 parts of fumed silica, 1-5 parts of carbon black, 50-80 parts of butyl acetate, 1-5 parts of methyl acrylate and 2-5 parts of n-decyl alcohol;
the particle size of the carbon black is between 10 and 50 nm.
Preferably, the preparation method of the matte slurry comprises the following steps: adding fumed silica, carbon black and methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 1-3h, adding n-decanol and butyl acetate after grinding, placing the mixture into a high-pressure reaction kettle, and reacting for 2-4 h at the temperature of 200-250 ℃ under the pressure of 3MPa to obtain the matte slurry.
The invention also provides a preparation method of the matte graphene coating, which comprises the following steps:
preparing matte slurry and graphene resin slurry, adding the matte slurry and the graphene resin slurry into a nano wear-resistant graphene coating containing polyurethane resin, a monomer, an additive and a photoinitiator, and fully stirring for 30-60min to obtain the matte graphene coating.
Compared with the prior art, the invention has the following beneficial effects:
(1) The matte graphene coating provided by the invention is simple in preparation method, local high temperature, high pressure, shock wave, microjet and other effects generated by infiltrating, dispersing and ultrasonic processing on graphene weaken acting force between graphene sheets, and raw material components and proportion are controlled, so that the prepared graphene epoxy coating has the characteristics of good adhesive force and high mechanical strength.
(2) According to the matte graphene coating provided by the invention, carbon black is added, so that fumed silica can be better dispersed under the action of high specific surface area of the carbon black, meanwhile, the fumed silica and graphite are broken by chemical bonds under the action of mechanical force to generate a new active surface with higher unsaturation degree, the lattice defects can be caused by the action of the mechanical force, the internal energy of solid matters is increased, and the solid matters are in an unstable chemical activity state, which is favorable for exciting chemical reactions. And then, by wet grinding, the powder slurry firstly generates a new surface with high activity, lattice defects and distortion are less generated, the agglomeration effect among the powder is weak, the powder is uniformly dispersed and has strong uniformity, the surface of a ground product is smooth and clean, and the grinding efficiency is obviously superior to that of dry grinding.
(3) According to the matte graphene coating provided by the invention, the surface of fumed silica is modified by using n-decanol, and the hydroxyl is replaced by alkoxy by using the dehydration reaction between the hydroxyl at the tail end of the n-decanol and the hydroxyl on the surface of the silica, so that the number of the same hydroxyl on the surface of the silica is effectively reduced, and the self-aggregation of the silica is inhibited.
(4) According to the matte graphene coating provided by the invention, the main coating base material is polyurethane resin, and meanwhile, the epoxy resin is added into the graphene resin slurry, so that the compatibility difference between the two polymers is utilized, and the surface glossiness of the coating can be reduced to a certain extent, so that the matte performance of the coating is improved.
(5) The matte graphene coating provided by the invention has the advantages of soft hand feeling and outstanding antifouling property.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the matte graphene coating specifically comprises the following steps:
(1) Preparing graphene resin slurry: uniformly mixing 30 parts of epoxy resin, 1 part of organic bentonite and 35 parts of ethanol, and then carrying out infiltration treatment on graphene; after the infiltration treatment is finished, adding 5 parts of polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
(2) Preparation of matte slurry: adding 25 parts of fumed silica, 1 part of carbon black and 1 part of methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 1h, adding 2 parts of n-decyl alcohol and 50 parts of butyl acetate after grinding is finished, placing the mixture into a high-pressure reaction kettle, and reacting for 2 hours at the temperature of 200 ℃ under the pressure of 3MPa to obtain the matte slurry;
(3) Preparing a matte graphene coating: and (2) adding the graphene resin slurry (20 parts) prepared in the step (1) and the matte slurry (15 parts) prepared in the step (2) into a nano wear-resistant graphene coating containing 10 parts of polyurethane resin, 15 parts of hydroxy acrylic acid, 0.5 part of dimethyl silicone oil and 5 parts of azobisisobutyronitrile, and fully stirring for 30min to obtain the matte graphene coating.
Example 2
The preparation method of the matte graphene coating specifically comprises the following steps:
(1) Preparing graphene resin slurry: uniformly mixing 35 parts of epoxy resin, 2 parts of organic bentonite and 38 parts of ethanol, and then carrying out infiltration treatment on graphene; after the infiltration treatment is finished, adding 7 parts of polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
(2) Preparation of matte slurry: adding 30 parts of fumed silica, 3 parts of carbon black and 3 parts of methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 1.5h, adding 3 parts of n-decanol and 60 parts of butyl acetate after grinding is finished, placing the mixture into a high-pressure reaction kettle, and reacting for 2.5 hours at the temperature of 220 ℃ under the pressure of 3MPa to obtain the matte slurry;
(3) Preparing a matte graphene coating: and (3) adding the graphene resin slurry (25 parts) prepared in the step (1) and the matte slurry (20 parts) prepared in the step (2) into a nano wear-resistant graphene coating containing 20 parts of polyurethane resin, 20 parts of butyl acrylate, 1 part of phenethyl alcohol oleate and 7 parts of benzoic ether, and fully stirring for 40min to obtain the matte graphene coating.
Example 3
The preparation method of the matte graphene coating specifically comprises the following steps:
(1) Preparing graphene resin slurry: uniformly mixing 45 parts of epoxy resin, 4 parts of organic bentonite and 41 parts of ethanol, and then carrying out infiltration treatment on graphene; after the infiltration treatment is finished, adding 9 parts of polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
(2) Preparation of matte slurry: adding 35 parts of fumed silica, 4 parts of carbon black and 4 parts of methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 2.5h, adding 4 parts of n-decanol and 70 parts of butyl acetate after grinding is finished, placing the mixture into a high-pressure reaction kettle, and reacting for 3 hours at the temperature of 240 ℃ under the pressure of 3MPa to obtain the matte slurry;
(3) Preparing a matte graphene coating: and (3) adding the graphene resin slurry (35 parts) prepared in the step (1) and the matte slurry (9 parts) prepared in the step (2) into a nano wear-resistant graphene coating containing 30 parts of polyurethane resin, 25 parts of epoxy acrylic acid, 1.5 parts of sodium carboxymethyl cellulose and 9 parts of benzophenone, and fully stirring for 50min to obtain the matte graphene coating.
Example 4
The preparation method of the matte graphene coating specifically comprises the following steps:
(1) Preparing graphene resin slurry: uniformly mixing 50 parts of epoxy resin, 5 parts of organic bentonite and 45 parts of ethanol, and then carrying out infiltration treatment on graphene; after the infiltration treatment is finished, adding 10 parts of polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
(2) Preparation of matte slurry: adding 40 parts of fumed silica, 5 parts of carbon black and 5 parts of methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 3 hours, adding 5 parts of n-decyl alcohol and 80 parts of butyl acetate after grinding is finished, placing the mixture into a high-pressure reaction kettle, and reacting for 4 hours at the temperature of 250 ℃ under the pressure of 3MPa to obtain the matte slurry;
(3) Preparing a matte graphene coating: and (2) adding the graphene resin slurry (40 parts) prepared in the step (1) and the matte slurry (25 parts) prepared in the step (2) into a nano wear-resistant graphene coating containing 35 parts of polyurethane resin, 30 parts of amino acrylic acid, 2 parts of polyethylene wax and 10 parts of benzophenone, and fully stirring for 60min to obtain the matte graphene coating.
Comparative example 1
The preparation method of the graphene coating specifically comprises the following steps:
(1) Preparing graphene resin slurry: uniformly mixing 30 parts of epoxy resin, 1 part of organic bentonite and 35 parts of ethanol, and then carrying out infiltration treatment on graphene; after the infiltration treatment is finished, adding 5 parts of polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
(2) Preparing a matte graphene coating: and (2) fully stirring the graphene resin slurry (20 parts) prepared in the step (1) for 30min in the nano wear-resistant graphene coating containing 10 parts of polyurethane resin, 5 parts of fumed silica, 20 parts of hydroxy acrylic acid, 0.5 part of dimethyl silicone oil and 8 parts of azobisisobutyronitrile, so as to obtain the graphene coating.
Comparative example 2
The preparation method of the graphene coating specifically comprises the following steps:
(1) Preparation of matte slurry: adding 25 parts of fumed silica, 1 part of carbon black and 1 part of methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 1h, adding 2 parts of n-decyl alcohol and 50 parts of butyl acetate after grinding is finished, placing the mixture into a high-pressure reaction kettle, and reacting at the temperature of 200-250 ℃ for 2-4 hours under the pressure of 3MPa to obtain the matte slurry;
(2) Preparing a matte graphene coating: and (2) adding the matte slurry (15 parts) prepared in the step (1) into a nano wear-resistant graphene coating containing 10 parts of polyurethane resin, 8.5 parts of graphene, 20 parts of hydroxy acrylic acid, 0.5 part of dimethyl silicone oil and 8 parts of azobisisobutyronitrile, and fully stirring for 30min to obtain the graphene coating.
The graphene coatings obtained in examples 1 to 4 and comparative examples 1 to 2 were subjected to gloss, adhesion, and mechanical property tests, and the gloss of the printed sample was measured by a 60-degree gloss meter according to the GB/T8807 standard, and the adhesion property was measured by GB/T9286-1998, and the impact resistance of the coating [ film thickness (70. + -.10) μm ] was measured on a 150mm X70 mm X1 mm steel plate by GB/T1732-1993 "paint film impact resistance measurement method", and a weight of 1kg was used. The specific test results are as follows:
from the above experimental results, it can be seen that the matte graphene coatings prepared in examples 1 to 4 have low gloss, high adhesion, good appearance, high impact resistance, and good stability.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The matte graphene coating is characterized by being prepared from the following raw materials in parts by weight:
the graphene resin slurry is prepared from the following raw materials in parts by weight: 30-50 parts of epoxy resin, 1-5 parts of organic bentonite, 35-45 parts of ethanol, 1-15 parts of graphene and 5-10 parts of polyvinylpyrrolidone;
the preparation method of the graphene resin slurry comprises the following steps:
uniformly mixing epoxy resin, organic bentonite and ethanol, and then performing infiltration treatment on graphene; after the infiltration treatment is finished, adding polyvinylpyrrolidone while stirring, then stirring at a high speed for 40min, and then performing ultrasonic dispersion for 30min to obtain stable graphene resin slurry;
the preparation method of the matte slurry comprises the following steps: adding fumed silica, carbon black and methyl acrylate into a ball mill for wet grinding at the rotating speed of 2500r/min for 1-3h, adding n-decanol and butyl acetate after grinding, placing the mixture into a high-pressure reaction kettle, and reacting for 2-4 h at the temperature of 200-250 ℃ under the pressure of 3MPa to obtain the matte slurry.
2. The matte graphene coating according to claim 1, which is prepared from the following raw materials in parts by weight:
3. the matte graphene coating according to claim 1, which is prepared from the following raw materials in parts by weight:
4. the matte graphene coating according to claim 1, wherein the monomer is one or more of acrylic acid and acrylate containing epoxy groups, hydroxyl groups, nitrile groups, carboxylic acid groups, ether groups, amino groups, amide groups, benzene rings, saturated rings, alkoxy groups, and silicon atoms.
5. The matte graphene coating according to claim 1, wherein the additive is one or more of dimethicone, phenethyl alcohol oleate, organosiloxane, polyether, sodium carboxymethyl cellulose, polyethylene glycol, polyvinyl alcohol, and polyethylene wax.
6. The matte graphene coating according to claim 1, wherein the photoinitiator is one or more of phosphazene, phosphazene salt, phosphazene oxide, azobisisobutyronitrile, azobisisovaleronitrile benzil ketal, benzoyl formate, benzophenone, and tertiary amine accelerators.
7. The matte graphene coating according to claim 1, wherein the matte slurry is prepared from the following raw materials in parts by weight: 25-40 parts of fumed silica, 1-5 parts of carbon black, 50-80 parts of butyl acetate, 1-5 parts of methyl acrylate and 2-5 parts of n-decanol;
the particle size of the carbon black is between 10 and 50 nm.
8. A method for preparing the matte graphene coating according to any one of claims 1 to 7, which is characterized by comprising the following steps:
preparing matte slurry and graphene resin slurry, adding the matte slurry and the graphene resin slurry into a nano wear-resistant graphene coating containing polyurethane resin, a monomer, an additive and a photoinitiator, and fully stirring for 30-60min to obtain the matte graphene coating.
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| US20150210885A1 (en) * | 2012-07-24 | 2015-07-30 | Akzo Nobel Coatings International B.V. | Matting Paste Composition |
| CN106221528A (en) * | 2016-08-26 | 2016-12-14 | 广东巴德士化工有限公司 | A kind of have the most smooth PU matte white finish of gloss and preparation method thereof |
| CN108219655B (en) * | 2017-12-21 | 2020-10-30 | 东莞市德禧金成电子有限公司 | Nano wear-resistant graphene crystal coating |
| CN109161040B (en) * | 2018-08-24 | 2021-06-11 | 桂林电器科学研究院有限公司 | Preparation method of matte black polyimide film with low pinhole incidence |
| CN111040582A (en) * | 2019-12-31 | 2020-04-21 | 新疆烯金石墨烯科技有限公司 | Graphene anticorrosive paint special for transformer shell and preparation method thereof |
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