CN115353793A - Heavy-duty anticorrosive paint based on few-layer graphene and preparation method and application thereof - Google Patents
Heavy-duty anticorrosive paint based on few-layer graphene and preparation method and application thereof Download PDFInfo
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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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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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
- C08K3/08—Metals
- C08K2003/0812—Aluminium
Abstract
The invention relates to the field of graphene, and discloses a heavy-duty anticorrosive coating based on few-layer graphene, and a preparation method and application thereof, wherein the few-layer graphene is prepared from graphite powder under mechanical stripping, the graphene anticorrosive coating is composed of a component A and a component B, and the component A comprises, by mass, 1 per thousand to 7% of few-layer graphene, 10 to 35% of epoxy resin, 1 to 3% of aluminum paste, 10 to 25% of solvent, 30 to 60% of filler, and the component B comprises 30 to 65% of solvent, 20 to 50% of amide curing agent, and 1 per thousand to 3% of epoxy curing accelerator. The preparation method comprises the steps of nano grinding and shearing stirring. The few-layer graphene provided by the invention has the characteristic of small size (1-5 mu m) and strong sealing performance, and the graphene anticorrosive coating has the characteristics of acid/alkali corrosion resistance, hydrogen sulfide corrosion resistance, high adhesion, strong salt mist/humidity resistance and the like, and can meet the corrosion resistance of various metal substrates.
Description
Technical Field
The invention relates to the field of graphene anticorrosive coatings, in particular to a few-layer graphene and graphene anticorrosive coating as well as a preparation method and application thereof.
Background
The anticorrosive coating can be divided into a conventional anticorrosive coating and a heavy anticorrosive coating, and the heavy anticorrosive coating needs to be capable of providing protection for metal substrates and the like under a harsher corrosion environment and can be maintained for a longer time than the conventional anticorrosive coating. Heavy duty anticorrosive coatings can be classified into epoxy resin paints, vinyl chloride paints, acrylic paints, fluorocarbon paints, alkyd paints, silicone high temperature resistant paints, solventless anticorrosive coatings, extra heavy duty anticorrosive coatings, and the like. The application field of the method is widely applied to various fields such as military industry, civil life and the like, such as novel ocean engineering, modern transportation, energy industry, large-scale industrial enterprises, municipal facilities and the like. In marine engineering, the annual loss due to corrosion of metals can be as high as billions of dollars, especially for marine production platforms, which are large steel structures fixed in the ocean and are subject to long-term pollution from the marine environment, and thus the requirements for heavy-duty anticorrosive coatings are extremely high. Acid, alkali, sulfide and the like in seawater are all the most aggressive to corrosion, more efforts are required for the research and development of anticorrosive materials in China, and the development of novel heavy anticorrosive coatings provides huge prospects and benefits for the economy and industry of domestic industries.
However, with the upgrading of high and new industries and technologies and the influence of global large environment, the market demand for heavy-duty anticorrosive coatings is changing continuously, and besides the basic requirements of high adhesion, chemical corrosion resistance, low film thickness and the like, the requirements of people for environmental protection (without zinc and lead) are increasing, so that the requirements are gradually the target direction of research and development and progress of heavy-duty anticorrosive coatings.
The coordination number of carbon atoms in the graphene is 3, the bond length between every two adjacent carbon atoms is 1.42 multiplied by 10-10 meters, and the included angle between bonds is 120 degrees. The honeycomb-type layered structure with hexagonal rings linked between carbon atoms is one of the known materials with extremely high strength. Graphene has given its special properties in many areas, while it is extremely impermeable. The modified epoxy resin is also proved to be used as an additive in the anticorrosive paint, thereby effectively blocking the contact of oxygen and water molecules and improving the anticorrosive performance of the paint. However, in many heavy-duty anticorrosive coatings with graphene added, modified graphene and large-sized graphene are mostly used, and meanwhile, many heavy metal components are also contained.
The performance of graphene has a certain relationship with the number of layers, and few-layer graphene (generally 3 to 10 layers of graphene) can improve the performance as an additive compared with multi-layer graphene (more than 10 layers).
Therefore, a method for efficiently obtaining few-layer graphene is developed, the graphene anticorrosive paint with better acid/alkali corrosion resistance, hydrogen sulfide corrosion resistance and high adhesion (more than or equal to 13 MPa) is prepared, and the graphene heavy anticorrosive paint with excellent comprehensive performance and no heavy metal belongs to the technical problem in the field.
Disclosure of Invention
The invention aims to provide an efficient preparation method of few-layer graphene, a green and environment-friendly (heavy metal-free) graphene heavy-duty anticorrosive coating with excellent comprehensive performance, and a preparation method and application thereof.
The graphene heavy-duty anticorrosive coating provided by the invention fully utilizes a shielding wall which is formed by dispersing few layers of graphene in the coating and is difficult to permeate, can prevent external oxygen, water vapor and other various corrosive gases and components from contacting with a metal substrate, radically stops the oxidation of the metal substrate, slows down the corrosion progress of metal, and provides long-acting and durable protection for the metal substrate.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing few-layer graphene, wherein the few-layer graphene is obtained by mechanically peeling off graphite powder, the method comprising the steps of:
step one, mixing graphite powder and water according to the proportion of 1,
and step two, carrying out high-speed shearing on the graphite powder dispersion liquid, wherein the rotating speed is not lower than 12000r/min, and the time is not less than 4h, so as to obtain the few-layer graphene dispersion liquid.
And thirdly, freeze-drying the obtained few-layer graphene dispersion liquid in a freeze dryer to obtain few-layer graphene powder.
In particular, the carbon element content of the few-layer graphene is 99.8% -99.95%.
In particular, the conductivity of the few-layer graphene is 1000S/m to 3000S/m.
In particular, the few-layer graphene has a radial dimension of 1 μm to 5 μm. (by transmission electron microscope and atomic force microscope)
Further, the temperature range of the first step is controlled to be 30-60 ℃.
The second aspect of the invention provides a graphene heavy-duty anticorrosive coating which is composed of a component A and a component B, wherein the component A comprises 1 per thousand-7% of few-layer graphene, 10-35% of epoxy resin and 1-3% of aluminum paste by mass percent, and the component B comprises 30-65% of solvent and 1 per thousand-3% of epoxy curing accelerator.
Further, the epoxy resin in the A component comprises 2-3 epoxy resins with an epoxy value of 0.4-0.6.
Further, the component B contains 30-50% of curing agent diethylenetriamine.
Furthermore, the component A also comprises 1-3% of an auxiliary agent, 10-30% of a solvent and 30-50% of a filler, wherein the auxiliary agent is selected from one or more of a leveling agent, a defoaming agent, a dispersing agent and a dehydrating agent, the filler is selected from one or more of titanium dioxide, barium sulfate, zinc oxide, bentonite, aluminium dihydrogen tripolyphosphate, talcum powder, carbon black and mica powder, and the solvent is selected from one or more of N-butyl acetate, propylene glycol methyl ether acetate, butanone, methyl isobutyl ketone, cyclohexanone, toluene, xylene, methanol, ethanol, ethylene glycol, isopropanol, glycerol, propylene glycol methyl ether, diethylene glycol ethyl ether acetate, diethylene glycol monobutyl ether, diethylene glycol butyl ether acetate, ethyl acetate and N-methylpyrrolidone.
The third aspect of the invention provides a preparation method of a heavy-duty anticorrosive coating based on few-layer graphene, which comprises the following steps:
step one, adding graphene, a filler, a dispersant and a solvent into a shear mixer according to a required ratio, and shearing at a high speed for not less than 30min at a rotating speed of not less than 2000rpm.
And step two, adding the epoxy resin in the proportion into the few-layer graphene in the step one, and grinding the graphene to the fineness of less than or equal to 40 microns by using a sand mill.
And step three, adding the aluminum paste with the proportion into the mixture obtained in the step two, and shearing at a high speed for not less than 30min to obtain the epoxy resin A component.
And step four, mixing and dispersing a curing agent, an epoxy curing accelerator and a solvent according to the required proportion to obtain the epoxy resin B component.
In the first step, the temperature needs to be controlled to be 30-55 ℃.
And the grinding medium of the sand mill used in the second step is zirconium beads with the diameter of 1.5-3 mm.
The rotating speed of the shearing dispersion in the third step is 1000rpm-1500rpm.
The fourth aspect of the invention provides the graphene heavy-duty anticorrosive paint prepared by the preparation method.
The fifth aspect of the invention provides an application of the graphene epoxy coating in crude oil storage tanks, ships, offshore platforms and offshore wind power plants.
The graphene epoxy coating provided by the invention has the advantages of strong adhesive force (more than or equal to 13 MPa), acid corrosion resistance (more than or equal to 6000H) and alkali corrosion resistance (more than or equal to 5 percent of H2 SO4), hydrogen sulfide corrosion resistance (more than or equal to 2000H) and no zinc, tin, aluminum and other metal substances, has strong neutral salt spray resistance (more than or equal to 4000H), small neutral film thickness (80-120 mu m), good brushing performance (no bubbling and no peeling), simple construction process (spraying and brushing), can meet the construction requirements of various metal substrates, and can provide comprehensive anti-corrosion protection for the metal substrates.
Description of the drawings:
fig. 1 is a transmission electron microscope and atomic force microscope image of the few-layer graphene obtained in example 1.
Fig. 2 is a schematic view of the few-layer graphene obtained in example 1.
Fig. 3 is a photograph of a sample after neutral salt spray experiment of the graphene epoxy coating in each example.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
The hydrogen sulfide corrosion resistance test of the graphene heavy-duty anticorrosive coating is carried out according to GB/T4157-2006, the salt spray test is carried out according to GB/T1771-2007, and the paint film adhesion test is carried out according to GB/T1720-1979. And cleaning treatment is carried out according to GB/T8923.1-2011 before the paint film is coated.
In the following examples and application examples, the room temperature is 25 ℃.
Example 1
(1) Mixing 1 part of graphite powder and 20 parts of water in a stirrer, keeping the temperature at 40 ℃ to obtain graphite powder dispersion liquid,
(2) And (3) shearing the graphite powder dispersion liquid obtained in the step (1) at a high speed in a stirring device, wherein the grinding medium of a sand mill is zirconium beads with the diameter of 1.5mm, the selected rotating speed is 12000r/min, and the time is 5h, so that the few-layer graphene dispersion liquid is obtained.
(3) And freezing the obtained few-layer graphene dispersion liquid at-10 ℃, and then freeze-drying in a freeze dryer to obtain corresponding few-layer graphene powder.
(4) Taking 2 parts of few-layer graphene powder, 0.5 part of a dispersing agent, 0.5 part of a defoaming agent, 1 part of bentonite, 5 parts of talcum powder, 3 parts of aluminium dihydrogen tripolyphosphate, 15 parts of barium sulfate, 30 parts of calcium carbonate and 25 parts of a solvent (a mixed solvent of n-butyl acetate, cyclohexanone, xylene, isopropanol and diethylene glycol monobutyl ether is used as a solution, the volume ratio is 10%:40%:30%:10%: 10%), sequentially adding the materials into a high-speed shearing mixer, adjusting the rotating speed to 2000rpm, and shearing and dispersing for 40min until all solids are uniformly dispersed and no layering occurs.
(5) And (3) adding 7 parts of E-51 type bisphenol A epoxy resin (with the epoxy value of 0.48-0.54) and 9 parts of E-44 type bisphenol A epoxy resin (with the epoxy value of 0.41-0.47) into the mixture obtained in the step (2), mechanically stirring, transferring into a sand mill, and grinding for 40min at the rotating speed of 500rpm.
(6) And (4) adding 2 parts of aluminum paste into the mixture obtained in the step (5), and shearing and dispersing at the rotating speed of 1500rpm for 30min to obtain the component A of the graphene heavy-duty anticorrosive coating.
(7) Taking 50 parts of diethylenetriamine curing agent, 0.5 part of epoxy curing accelerator and 42 parts of solvent (the solution is a mixed solvent of diethylene glycol ethyl ether acetate, xylene, ethyl acetate and N-methylpyrrolidone, the volume ratio is 20 percent to 40 percent to 20 percent), and mechanically stirring uniformly to obtain the graphene epoxy coating B component.
(8) After the component A and the component B of the graphene heavy-duty anticorrosive paint are uniformly mixed according to the mass ratio of 5. The paint film in all the embodiments of the invention adopts a two-time spraying process, the two-time spraying interval is 2 hours, and the thickness of the paint film is 100 mu m.
Example 2
The few-layer graphene powder in example 1 is changed to 1 part, and the rest of the operation steps are unchanged.
Example 3
The few-layer graphene powder in example 1 was changed to 3 parts, and the remaining operation steps were unchanged.
In the case of the example 4, it is preferred,
the aluminum paste in example 1 was changed to 0.5 part, and the remaining operation steps were unchanged.
Example 5
The aluminum paste in example 1 was changed to 1 part, and the remaining operation steps were unchanged.
Example 6
The few-layer graphene powder in example 1 is changed to 0 part, and the rest of the operation steps are unchanged.
FIG. 1 is a transmission electron microscope and atomic force microscope image of the few-layer graphene obtained in example 1, showing that the radial dimension of the prepared few-layer graphene is about 1 μm to 5 μm,
fig. 2 is a schematic view of the few-layer graphene obtained in example 1, which is a fluffy black powder.
Fig. 3 is a photograph of a sample after neutral salt spray experiment of the graphene epoxy coating in each example, and it can be seen from the photograph that after 500 hours, the sample containing few layers of graphene has no rust spots and no bubbling, only the scribed lines have corrosion traces, and the corrosion does not expand the lines to both sides, and meets the requirements of GB/T1771-2007.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The graphene heavy-duty anticorrosive coating is composed of a component A and a component B, wherein the component A is composed of 1 per thousand-7% of few-layer graphene, 10% -35% of epoxy resin and 1% -3% of aluminum paste according to mass percentage, and the component B is composed of 30% -65% of solvent and 1 per thousand-3% of epoxy curing accelerator.
2. The heavy-duty anticorrosive coating based on few-layer graphene according to claim 1, wherein the few-layer graphene is prepared by the following steps:
firstly, mixing graphite powder and water according to the proportion of 1;
secondly, placing the graphite powder dispersion liquid in a high-speed shearing machine, wherein the rotating speed is not lower than 12000rpm, and the time is not less than 4h, so as to obtain a few-layer graphene dispersion liquid;
and step three, carrying out freeze-drying on the few-layer graphene dispersion liquid to obtain few-layer graphene powder.
3. The low-graphene-based heavy-duty coating of claim 2, wherein the low-graphene has a size of about 1 μm to about 5 μm as measured by transmission electron microscopy and atomic force microscopy.
4. The few-layer graphene-based heavy-duty anticorrosive coating of claim 2, wherein the temperature is controlled in the range of 30-60 ℃ in the first step.
5. The few-layer graphene-based heavy-duty anticorrosive coating according to claim 1, wherein the epoxy resin in the A component comprises 2 to 3 epoxy resins having an epoxy value of 0.4 to 0.6.
6. The heavy-duty anticorrosive coating based on few-layer graphene according to claim 1, wherein the component B contains 30% -50% of curing agent diethylenetriamine.
7. The heavy-duty paint based on few-layer graphene as claimed in claim 1, characterized in that the component a further comprises 1% -3% of an auxiliary agent, 10% -30% of a solvent, and 30% -50% of a filler, wherein the auxiliary agent is selected from one or more of a leveling agent, an antifoaming agent, a dispersing agent, and a dehydrating agent, the filler is selected from one or more of titanium dioxide, barium sulfate, zinc oxide, bentonite, aluminum dihydrogen tripolyphosphate, talc, carbon black, and mica powder, and the solvent is selected from one or more of N-butyl acetate, propylene glycol methyl ether acetate, methyl isobutyl ketone, cyclohexanone, toluene, xylene, methanol, ethanol, ethylene glycol, isopropanol, glycerol, propylene glycol methyl ether, diethylene glycol ethyl ether acetate, diethylene glycol monobutyl ether, diethylene glycol butyl ether acetate, ethyl acetate, and N-methylpyrrolidone.
8. The preparation method of the heavy-duty paint based on the few-layer graphene as claimed in any one of claims 1 to 7, is characterized by comprising the following steps:
step one, adding graphene, a filler, a dispersant and a solvent into a shear mixer according to a required ratio, and shearing at a high speed for not less than 30min at a rotating speed of not less than 2000rpm.
And step two, adding the epoxy resin in the proportion into the few-layer graphene in the step one, and grinding the graphene to the fineness of less than or equal to 40 micrometers by using a sand mill.
And step three, adding the aluminum paste with the ratio into the mixture obtained in the step two, and shearing at a high speed for not less than 30min to obtain the epoxy resin A component.
And step four, mixing and dispersing a curing agent, an epoxy curing accelerator and a solvent according to the required proportion to obtain the epoxy resin B component.
9. The preparation method of the heavy-duty anticorrosive paint based on few-layer graphene according to claim 8, characterized in that, in the first step, the temperature is controlled to be 30-55 ℃; the grinding medium of the sand mill used in the second step is zirconium beads with the diameter of 1.5 mm-3 mm; the rotating speed of the shearing dispersion in the third step is 1000rpm-1500rpm.
10. Use of the heavy anticorrosive coating based on few-layer graphene according to any one of claims 1 to 7 in steel structures, crude oil storage tanks, ships, offshore platforms, offshore wind power plants.
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