CN111978771A - Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method - Google Patents
Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method Download PDFInfo
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- CN111978771A CN111978771A CN201910424940.6A CN201910424940A CN111978771A CN 111978771 A CN111978771 A CN 111978771A CN 201910424940 A CN201910424940 A CN 201910424940A CN 111978771 A CN111978771 A CN 111978771A
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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
- 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
- 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
- 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 relates to the technical field of coatings, and particularly discloses a modified graphene oxide, a preparation method thereof, an anticorrosive coating containing the modified graphene oxide and a preparation method of the anticorrosive coating. The anticorrosive paint comprises the following raw material components in parts by weight: 50-150 parts of water-based resin; 0.5-1 part of modified graphene oxide; 50-200 parts of a curing agent. The anticorrosive coating provided by the invention is prepared from the modified graphene serving as a filler and the water-based resin, and the corrosion resistance and the mechanical strength of the anticorrosive coating are improved by utilizing the good dispersibility, small-size effect and two-dimensional structure of the modified graphene and the crosslinking and curing effect among the polyglycerol modified graphene, the water-based resin and the curing agent.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a modified graphene oxide, a preparation method thereof, an anticorrosive coating containing the modified graphene oxide and a preparation method of the anticorrosive coating.
Background
The economic loss caused by corrosion is quite remarkable and occupies 3-5% of GDP, so that the anticorrosive paint becomes a paint which is widely applied in the fields of modern industry, traffic, energy, ocean engineering and the like. After the surface of the material is coated with the anticorrosive paint, the invasion of a substrate by various corrosive media can be effectively inhibited or delayed, the service life of the material is prolonged, and the economic cost is saved.
At present, the zinc-rich and flaky graphite heavy corrosion protection which is most widely applied is difficult to meet the performance requirements of modern or future corrosion protection. The zinc-rich anticorrosive paint has limited zinc resource and heavy zinc compound has great harm to environment, and the flaky graphite has unsmooth and great brittleness caused by the thickness of the sheet layer. In addition, the existing anticorrosive paint containing graphene also has the problems of environmental pollution, high cost, poor dispersion stability of graphene and the like. Therefore, the development of new anticorrosion inhibitors and the improvement of the overall properties of the coating are at hand.
Disclosure of Invention
Aiming at the problems of insufficient anticorrosive performance, easy environmental pollution, poor dispersion stability of graphene and the like of the existing anticorrosive paint, the invention provides modified graphene oxide, a preparation method thereof, an anticorrosive paint containing the modified graphene oxide and a preparation method thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a modified graphene oxide is modified by grafting polyglycerol on the surface of graphene oxide. The modified graphene oxide has a large number of hydroxyl functional groups on the surface, so that the graphene oxide has good dispersibility, maintains the small-size effect and the two-dimensional structure of the graphene oxide, can be stably dispersed in a coating and is crosslinked and cured with water-based resin to form a paint film, the mechanical strength, the wear resistance and the corrosion resistance of the paint film are improved, and the service life of the material is prolonged.
In addition, the polyglycerol modified graphene oxide has better dispersibility and stability in the coating, due to the small-size effect and the two-dimensional structure of the polyglycerol modified graphene oxide, the polyglycerol modified graphene oxide is uniformly filled in holes of a coating film of the coating, the layers are stacked to form a compact physical isolation layer, due to the surface effect of the graphene oxide, the graphene oxide has poor wettability to water, water molecules can be prevented from contacting a metal matrix through the coating, and therefore corrosion is reduced. Meanwhile, the polyglycerol modified graphene oxide has a strong conductive effect, so that electrons lost by anodic reaction on the metal surface can be quickly transferred to the coating surface through the graphene sheet layer, cathode electrons directly react with the coating surface, and generated OH-The metal ions stay on the surface of the coating layer and cannot be precipitated, and the metal ions of the anode are accumulated continuously to inhibit the anode reaction, so that the corrosion of the metal is slowed down. The graphene structure in the polyglycerol modified graphene oxide can be passivated with metal to form a protective film, so that the protective capability of the coating is enhanced, and the corrosion resistance of the coating is further improved.
The invention also provides a preparation method of the modified graphene oxide, which comprises the following steps of mixing the raw materials in a mass-volume ratio of 8-50 mg: 1mL of graphene oxide reacts with glycidol to obtain the modified graphene oxide.
Further, the reaction temperature of the graphene oxide and glycidol is 100-180 ℃, the reaction time is 2-48 hours, the reaction is fully carried out, and polyhydroxylation modification is carried out on the graphene oxide.
Further, after the reaction of the graphene oxide and glycidol is finished, adding the system to methanol to obtain a mixed solution after the system is cooled to room temperature, adding the mixed solution to acetone to perform precipitation treatment, filtering and drying to obtain the polyglycerol-modified graphene oxide.
Further, the graphene oxide is treated by potassium methoxide and then reacts with glycidol, and the treatment method comprises the following steps: uniformly mixing the graphene oxide with a saturated potassium methoxide solution, and refluxing at 60-90 ℃ for 1-24 hours.
Further, after the reflux is finished, repeatedly washing with methanol to remove potassium methoxide, and distilling under reduced pressure to remove the methanol solvent to obtain deprotonated graphene oxide, wherein the deprotonated graphene oxide can provide an alkaline environment in a reaction system, so that the ring opening of glycidol epoxy is facilitated, and the reaction of the graphene oxide and glycidol is facilitated to form the polyglycerol modified graphene oxide.
The invention also provides an anticorrosive paint which comprises the modified graphene oxide.
Further, the anticorrosive paint comprises the following raw material components in parts by weight:
50-150 parts of water-based resin; 0.5-1 part of modified graphene oxide; 50-200 parts of a curing agent.
Further, the water-based resin is at least one of water-based unsaturated polyester resin, water-based vinyl resin, water-based epoxy resin, water-based phenolic resin, water-based amino resin, water-based polyurethane resin, water-based alkyd resin, water-based acrylic resin or water-based polyimide resin; the curing agent is at least one of aliphatic amine curing agent, alicyclic amine curing agent, polyamide curing agent, amino resin curing agent or aliphatic amine adduct, the curing agent, water-based resin and modified graphene oxide form a paint film through crosslinking curing (condensation, ring closure, addition or catalysis and other chemical reactions), meanwhile, nitrogen elements in the curing agent and metal form hydrogen bonds, so that the adhesive force and the corrosion and rust resistance of the paint film are further improved, and in addition, the modified graphene oxide and the water-based resin are matched for use, so that the salt fog resistance, the acid and alkali resistance of the paint film are improved, the hardness of the paint film is high, and the flexibility is good.
Furthermore, the anticorrosive paint also comprises an auxiliary agent for improving the performance of the paint, wherein the auxiliary agent comprises at least one of a defoaming agent, a drier, a thickening agent, a leveling agent, a film-forming auxiliary agent, an anti-skinning agent, a mildew-proof agent or a wetting agent.
The invention also provides a preparation method of the anticorrosive paint, which comprises the following steps:
(1) dispersing polyglycerol modified graphene in a solvent to obtain a dispersion liquid with the concentration of 0.1-10 mg/ml, adding the aqueous resin, and uniformly stirring to obtain a viscous liquid;
(2) adding a diluent which is 4-6 times of the mass of the water-based resin into the viscous liquid to prepare slurry;
(3) and adding a curing agent into the slurry, and uniformly stirring to obtain the anticorrosive paint.
Further, in the step (1), the solvent is water or a mixture of water and at least one of organic solvents miscible with water in any proportion; in the step (2), the diluent is at least one of water and the organic solvent.
Further, the organic solvent is methanol, ethanol, ethylene glycol, glycerol, acetone or diglyme, so that the modified graphene oxide is uniformly dispersed in the coating.
Further, in the step (1), the stirring speed is 3000-6000 rpm, and the time is 45-75 min; in the step (3), the stirring speed is 3000-6000 rpm, and the stirring time is 5-15 min.
Compared with the prior art, the technical scheme provided by the invention can be used for obtaining the polyglycerol modified graphene with good dispersibility, the polyglycerol modified graphene is used as the filler and the water-based resin to prepare the anticorrosive coating, and the good dispersibility, small-size effect and two-dimensional structure of the polyglycerol modified graphene and the cross-linking and curing effect among the polyglycerol modified graphene, the water-based resin and the curing agent are utilized to improve the corrosion resistance, mechanical strength and wear resistance of the anticorrosive coating. Meanwhile, the method has the advantages of simple process, mild conditions, environmental protection, low cost and convenient operation.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The modified graphene oxide is prepared by reacting 0.8g of graphene oxide with 100mL of glycidol, and the preparation method specifically comprises the following steps:
(1) stirring and uniformly mixing graphene oxide and 50mL of saturated potassium methoxide solution at 15 ℃ for 3h, refluxing at 90 ℃ for 1h, repeatedly washing with methanol to remove potassium methoxide, and distilling under reduced pressure to remove the methanol solvent to obtain deprotonated graphene oxide;
(2) mixing deprotonated graphene oxide with glycidol, reacting for 48 hours at 100 ℃ in a nitrogen atmosphere, after the reaction is finished, cooling the system to room temperature, adding the cooled system to 80mL of methanol to obtain a mixed solution, adding the mixed solution to sufficient acetone (the amount of the acetone can meet the precipitation requirement), carrying out precipitation treatment, filtering, and drying to obtain the polyglycerol-modified graphene oxide A.
Example 2
The modified graphene oxide is prepared by reacting 1g of graphene oxide with 70mL of glycidol, and the preparation method specifically comprises the following steps:
(1) Stirring graphene oxide and 40mL of saturated potassium methoxide solution at 30 ℃ for 0.5h, uniformly mixing, refluxing at 80 ℃ for 6h, repeatedly washing with methanol, removing potassium methoxide, and removing the methanol solvent by reduced pressure distillation to obtain deprotonated graphene oxide;
(2) mixing deprotonated graphene oxide with glycidol, reacting for 4 hours at 150 ℃ in a nitrogen atmosphere, after the reaction is finished, cooling the system to room temperature, adding the cooled system to 60mL of methanol to obtain a mixed solution, adding the mixed solution to sufficient acetone (the amount of the acetone can meet the precipitation requirement), carrying out precipitation treatment, filtering, and drying to obtain polyglycerol-modified graphene oxide B.
Example 3
The modified graphene oxide is prepared by reacting 5g of graphene oxide with 100mL of glycidol, and the preparation method specifically comprises the following steps:
(1) stirring graphene oxide and 60mL of saturated potassium methoxide solution at 15-30 ℃ for 0.5-3 h, uniformly mixing, refluxing at 60 ℃ for 24h, repeatedly washing with methanol, removing potassium methoxide, and removing the methanol solvent by reduced pressure distillation to obtain deprotonated graphene oxide;
(2) mixing deprotonated graphene oxide with glycidol, reacting at 180 ℃ for 2h in a nitrogen atmosphere, after the reaction is finished, cooling the system to room temperature, adding the cooled system to 90mL of methanol to obtain a mixed solution, adding the mixed solution to sufficient acetone (the amount of the acetone can meet the precipitation requirement), carrying out precipitation treatment, filtering, and drying to obtain polyglycerol-modified graphene oxide C.
Example 4
The anticorrosive paint comprises the following raw material components in parts by weight:
50 parts of water-based epoxy resin; 0.5 part of polyglycerol-modified graphene oxide A; and 50 parts of a polyamide curing agent.
The preparation method of the anticorrosive paint comprises the following steps:
(1) dispersing the polyglycerol modified graphene A in water to obtain a dispersion liquid with the concentration of 10mg/ml, adding water-based epoxy resin, and stirring at 3000rpm for 75min to obtain a viscous liquid;
(2) adding water with the mass 6 times that of the waterborne epoxy resin into the viscous liquid as a diluent to prepare slurry;
(3) and adding a polyamide curing agent into the slurry, and stirring at 6000rpm for 5min to obtain the anticorrosive coating.
Example 5
The anticorrosive paint comprises the following raw material components in parts by weight:
150 parts of water-based epoxy resin; 1 parts of polyglycerol-modified graphene oxide B; 200 parts of polyamide curing agent.
The preparation method of the anticorrosive paint comprises the following steps:
(1) dispersing polyglycerol modified graphene B in a solvent formed by mixing water and methanol in equal volume to obtain a dispersion liquid with the concentration of 0.1mg/ml, adding waterborne epoxy resin, and stirring at 4500rpm for 60min to obtain a viscous liquid;
(2) adding ethanol with the mass 4 times that of the waterborne epoxy resin into the viscous liquid as a diluent to prepare slurry;
(3) And adding a polyamide curing agent into the slurry, and stirring at 4500rpm for 10min to obtain the anticorrosive coating.
Example 6
The anticorrosive paint comprises the following raw material components in parts by weight:
100 parts of water-based epoxy resin; 0.8 part of polyglycerol-modified graphene oxide C; 120 parts of a mixture of a fatty amine curing agent and a polyamide curing agent in equal proportion.
The preparation method of the anticorrosive paint comprises the following steps:
(1) dispersing the polyglycerol modified graphene C in a mixed solvent with the volume ratio of water to ethanol being 2:1 to obtain a dispersion liquid with the concentration of 5mg/ml, adding aqueous epoxy resin, and stirring at 6000rpm for 45min to obtain a viscous liquid;
(2) adding water with the mass 5 times that of the waterborne epoxy resin into the viscous liquid as a diluent to prepare slurry;
(3) and adding a mixture of a fatty amine curing agent and a polyamide curing agent in equal proportion into the slurry, and stirring at 3000rpm for 15min to obtain the anticorrosive coating.
Example 7
The anticorrosive paint comprises the following raw material components in parts by weight:
50 parts of water-based acrylic resin; 0.5 part of polyglycerol-modified graphene oxide B; 50 parts of amino resin curing agent.
The preparation method of the anticorrosive paint comprises the following steps:
(1) Dispersing the polyglycerol modified graphene B in water to obtain a dispersion liquid with the concentration of 3mg/ml, adding water-based acrylic resin, and stirring at 6000rpm for 45min to obtain a viscous liquid;
(2) adding water with the mass 5 times that of the water-based acrylic resin into the viscous liquid as a diluent to prepare slurry;
(3) and adding an amino resin curing agent into the slurry, and stirring at 6000rpm for 6min to obtain the anticorrosive paint.
The anticorrosive paint provided in the above embodiment may further include conventional additives for improving the performance of the paint, including a defoaming agent, a drier, a thickener, a leveling agent, a film-forming additive, an anti-skinning agent, a mildew preventive or a wetting agent, and the like.
In order to better illustrate the technical solution of the present invention, further comparison is made below by means of a comparative example and an example of the present invention.
Comparative example 1
The polyglycerol-modified graphene oxide B in example 5 was changed to conventional unmodified graphene oxide, and the other components and the preparation method were the same as those in example 5, to obtain an anticorrosive coating.
In order to better illustrate the characteristics of the anticorrosive coatings provided by the examples of the present invention, the anticorrosive coatings prepared in example 5 and comparative examples 1 and 2 were tested for their respective properties, and the results are shown in table 1.
TABLE 1
According to the data, the anticorrosive coating provided by the embodiment of the invention has the advantages of high film hardness, good flexibility, strong adhesion, excellent salt spray resistance, acid and alkali resistance and aging resistance, and no foaming, softening and swelling on the surface of a coating film after the salt spray resistance, acid and alkali resistance and aging resistance are tested in a specified test time; the coating film does not foam or flow after a specified test time in the heat aging resistance test. In addition, the paint film color of the anticorrosive paint provided by the embodiment of the invention is uniform and consistent with the appearance surface tone, no particles, pinholes, bubbles or wrinkles exist, the grid test is less than or equal to level 1, the bending property is less than or equal to 10mm, the impact resistance is more than or equal to 30cm, and the performance parameters meet or even are superior to the national standard. The anticorrosive coatings in examples 4, 6 and 7 of the present invention have the effect equivalent to that of the anticorrosive coating in example 5.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A modified graphene oxide characterized by: the method is characterized in that polyglycerol is grafted on the surface of graphene oxide for modification.
2. The method for producing a modified graphene oxide according to claim 1, wherein: mixing 8-50mg of: 1mL of graphene oxide reacts with glycidol to obtain the modified graphene oxide.
3. The method for preparing modified graphene oxide according to claim 2, wherein: the reaction temperature of the graphene oxide and the glycidol is 100-180 ℃, and the reaction time is 2-48 h.
4. The method for preparing the modified graphene oxide according to claim 3, wherein the graphene oxide is treated by potassium methoxide and then reacts with glycidol, and the treatment method comprises the following steps: uniformly mixing the graphene oxide with a saturated potassium methoxide solution, and refluxing at 60-90 ℃ for 1-24 hours.
5. An anticorrosive paint is characterized in that: comprising the modified graphene oxide as claimed in any one of claims 1 to 4.
6. The anticorrosive paint as claimed in claim 5, which comprises the following raw materials in parts by weight:
50-150 parts of water-based resin; 0.5-1 part of modified graphene oxide; 50-200 parts of a curing agent.
7. The anticorrosive paint according to claim 6, wherein the aqueous resin is at least one of an aqueous unsaturated polyester resin, an aqueous vinyl resin, an aqueous epoxy resin, an aqueous phenol resin, an aqueous amino resin, an aqueous polyurethane resin, an aqueous alkyd resin, an aqueous acrylic resin or an aqueous polyimide resin; the curing agent is at least one of aliphatic amine curing agent, alicyclic amine curing agent, polyamide curing agent, amino resin curing agent or aliphatic amine adduct.
8. A method for preparing the anticorrosive paint of claim 6 or 7, characterized by comprising the following steps:
(1) dispersing polyglycerol modified graphene oxide in a solvent to obtain a dispersion liquid with the concentration of 0.1-10 mg/ml, adding the aqueous resin, and uniformly stirring to obtain a viscous liquid;
(2) adding a diluent which is 4-6 times of the mass of the water-based resin into the viscous liquid to prepare slurry;
(3) and adding a curing agent into the slurry, and uniformly stirring to obtain the anticorrosive paint.
9. The method for preparing an anticorrosive paint according to claim 8, characterized in that: in the step (1), the solvent is water or a mixture of water and at least one of organic solvents miscible with water in any proportion; in the step (2), the diluent is at least one of water and the organic solvent.
10. The method for preparing an anticorrosive paint according to claim 9, characterized in that: the organic solvent is methanol, ethanol, glycol, glycerol, acetone or diglyme.
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| CN112876925A (en) * | 2021-03-11 | 2021-06-01 | 国家电网有限公司 | Preparation method of low-temperature-resistant stretch-resistant anticorrosive paint |
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| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
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| CN114736583A (en) * | 2022-04-20 | 2022-07-12 | 湖南隆盛达钢管制造有限公司 | Corrosion-resistant preparation process of spiral steel pipe |
| CN114921145A (en) * | 2022-06-10 | 2022-08-19 | 洛阳大豫实业有限公司 | Modified graphene anticorrosive paint and preparation method thereof |
| CN115322607A (en) * | 2022-09-06 | 2022-11-11 | 安徽新大陆特种涂料有限责任公司 | Chlorinated polyester alloy heat-resistant anticorrosive paint and preparation process thereof |
| CN115322607B (en) * | 2022-09-06 | 2023-10-13 | 安徽新大陆特种涂料有限责任公司 | Chlorinated polyester alloy heat-resistant anticorrosive paint and preparation process thereof |
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