CN114958102A - Bottom surface integrated composite coating and preparation method and coating method thereof - Google Patents
Bottom surface integrated composite coating and preparation method and coating method thereof Download PDFInfo
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- CN114958102A CN114958102A CN202210717227.2A CN202210717227A CN114958102A CN 114958102 A CN114958102 A CN 114958102A CN 202210717227 A CN202210717227 A CN 202210717227A CN 114958102 A CN114958102 A CN 114958102A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 121
- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/002—Processes for applying liquids or other fluent materials the substrate being rotated
- B05D1/005—Spin coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention provides a bottom surface integrated composite coating, a preparation method and a coating method thereof, relating to the technical field of industrial coatings. The bottom surface integrated composite coating provided by the invention comprises a component A and a component B which are independently subpackaged; the component A is prepared from 0-5% of modified graphene, 50-70% of fluorocarbon resin, 4-10% of epoxy resin, 0-30% of titanium dioxide, 0.2-1.0% of dispersing agent, 0.6-1.8% of organic soil, 10-20% of organic solvent, 0.2-0.5% of defoaming agent and 0-0.4% of flatting agent by mass percentage; the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene; the component B is an isocyanate curing agent; the mass ratio of the component A to the component B is 100:10 to 20. The bottom surface integrated composite coating provided by the invention has excellent performance, the preparation method is simple and efficient, and the coating can be coated in one step and cured at room temperature, so that the coating has a wide application prospect.
Description
Technical Field
The invention relates to the technical field of industrial coatings, in particular to a bottom surface integrated composite coating, a preparation method and a coating method thereof.
Background
With the development of economy and society, surface abrasion and corrosion of metals, buildings, woodware and the like are inevitably a critical problem. The common method at present is to coat three different organic coatings, namely a primer, a middle paint and a top paint on the surface of the material to prevent abrasion and corrosion. Epoxy resin is widely used as a primer of a coating due to good adhesive force, fluorocarbon resin (FEVE) coating has the performances of very superior wear resistance, corrosion resistance, weather resistance, stain resistance and the like compared with other coatings, and is frequently used as a finish protective coating in the coating to prolong the service life of the material. However, the common multi-layer and multi-step coating process for coating the primer, the intermediate paint and the finish paint has complex and tedious forming and curing process and long construction time, and the use efficiency of the paint is seriously influenced. Therefore, it is urgently needed to develop a simple and economical composite coating to overcome the above defects and achieve excellent anti-abrasion and anti-corrosion protection effects. The composite coating with the integrated bottom surface can improve the construction efficiency, has excellent wear resistance and corrosion resistance, and becomes one of the most effective protection strategies at present. However, the integrally-ground composite coating researched at present still has the problems of poor stability, high-temperature crosslinking in the preparation process, unobvious performance in the aspects of mechanics, friction and corrosion, and the like.
CN114410224A discloses a heavy-duty anticorrosive primer-topcoat coating based on epoxy grafted fluorocarbon resin and a preparation method thereof, wherein the coating comprises: the paint comprises a component A, 30-40% of epoxy grafted fluorocarbon resin, 0.2-1% of dispersing agent, 0.2-0.5% of defoaming agent, 0.6-1% of organic bentonite, 0.2-0.6% of fumed silica, 5-15% of rusty antirust pigment, 30-40% of zinc powder, 0-2% of fullerene, 2-5% of titanium dioxide, 0.2-0.5% of wetting agent, 0.1-0.3% of drier, 0.3-0.8% of ultraviolet absorber and 5-15% of mixed solvent; the component B comprises 40-60% of isocyanic acid curing agent, 40-60% of butyl ester and 0.5-1% of dehydrating agent, and the component A and the component B are mixed to obtain the heavy-duty anticorrosion primer-topcoat integrated coating. However, the coating provided by the technical scheme needs to be heated at high temperature for a long time in the epoxy grafting fluorocarbon process, the preparation process is complex, and the impact and hardness improvement effects are not obvious.
Disclosure of Invention
The invention aims to provide a bottom surface integrated composite coating, a preparation method and a coating method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a bottom surface integrated composite coating, which comprises an A component and a B component which are independently subpackaged;
the component A is prepared from 0-5% of modified graphene, 50-70% of fluorocarbon resin, 4-10% of epoxy resin, 0-30% of titanium dioxide, 0.2-1.0% of dispersing agent, 0.6-1.8% of organic soil, 10-20% of organic solvent, 0.2-0.5% of defoaming agent and 0-0.4% of flatting agent by mass percentage; the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene;
the component B is an isocyanate curing agent;
the mass ratio of the component A to the component B is 100:10 to 20.
Preferably, the fluorocarbon resin is hydroxyl FEVE resin, and the hydroxyl value is 40-100 mg KOH/g; the mass ratio of the fluorocarbon resin to the epoxy resin is 95-70: 5 to 30.
Preferably, the preparation method of the fluorinated graphene comprises the following steps: mixing graphite fluoride and an ethanol solution containing a stabilizer, and performing ultrasonic dispersion to obtain a graphite fluoride dispersion liquid; and shearing and stripping the graphite fluoride dispersion liquid at a high speed to obtain the fluorinated graphene.
Preferably, the stabilizer is polyvinylpyrrolidone; the concentration of the stabilizer in the ethanol solution containing the stabilizer is 5-15 mg/mL; the shearing speed of the high-speed shearing stripping is 5000-20000 r/min, and the time is 5-15 h; the concentration of the graphite fluoride in the graphite fluoride dispersion liquid is 0.4-3.2 mg/mL.
Preferably, the mass ratio of the fluorinated graphene to the zirconium phosphate in the zirconium phosphate modified fluorinated graphene is 0.5-1: 0.25 to 2.
Preferably, the preparation method of the zirconium phosphate modified fluorinated graphene comprises the following steps: mixing fluorinated graphene, dopamine and Tris buffer solution to obtain mixed solution; and carrying out solid-liquid separation on the mixed solution, and drying the obtained solid to obtain the zirconium phosphate modified fluorinated graphene.
The invention provides a preparation method of the bottom surface integrated composite coating, which comprises the following steps:
mixing the preparation raw materials of the component A to obtain a component A;
when in use, the component A and the component B are mixed to obtain the bottom surface integrated composite coating.
Preferably, the preparation raw material mixing of the A component comprises the following steps:
carrying out first mixing on modified graphene and an organic solvent to obtain a modified graphene dispersion liquid;
carrying out second mixing on the modified graphene dispersion liquid and epoxy resin to obtain epoxy resin dispersion liquid;
thirdly mixing the epoxy resin dispersion liquid and fluorocarbon resin to obtain composite resin dispersion liquid;
and fourthly mixing the composite resin dispersion liquid, titanium dioxide, a dispersing agent, organic soil, a defoaming agent and a flatting agent to obtain the component A.
The invention provides a coating method of a bottom surface integrated composite coating, which comprises the steps of coating the bottom surface integrated composite coating or the bottom surface integrated composite coating prepared by the preparation method of the technical scheme on the surface of a substrate in one step, and curing at room temperature to obtain the composite coating.
Preferably, the one-step coating mode comprises blade coating, spin coating or spray coating; the room temperature curing time is 8-36 h.
The invention provides a bottom surface integrated composite coating, which comprises an A component and a B component which are independently subpackaged; the component A is prepared from 0-5% of modified graphene, 50-70% of fluorocarbon resin, 4-10% of epoxy resin, 0-30% of titanium dioxide, 0.2-1.0% of dispersing agent, 0.6-1.8% of organic soil, 10-20% of organic solvent, 0.2-0.5% of defoaming agent and 0-0.4% of flatting agent by mass percentage; the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene; the component B is an isocyanate curing agent; the mass ratio of the component A to the component B is 100:10 to 20. According to the invention, the epoxy resin and the fluorocarbon resin are simply mixed to prepare the bottom surface integrated composite coating, partial hydroxyl or carboxyl can be introduced into the composite coating by adding the epoxy resin (EP), so that the reaction activity is improved, the crosslinking density between coatings is increased, the adhesive force between the composite coating and substrates such as metal, buildings, woodware and the like is improved by utilizing the good adhesive property of the EP, and the wear resistance and corrosion resistance of the bottom surface integrated composite coating are improved. Preferably, the fluorinated graphene with the same C-F bond is added into the bottom surface integrated composite coating, so that the fluorinated graphene is uniformly dispersed in the composite coating and fully exerts the excellent lubricating property and the sheet layer barrier anticorrosion effect. The bottom surface integrated composite coating provided by the invention has excellent mechanical, antifriction, wear-resistant and corrosion-resistant properties, the preparation method is simple and efficient, the coating can be carried out on the surface of a substrate in one step, and the coating can be cured at room temperature, and the coating has wide application prospects in the industries of materials, machinery and the like.
Drawings
FIG. 1 is a graph of corrosion resistance of composite coatings prepared in example 1 and comparative example 1;
FIG. 2 is a graph of corrosion resistance of composite coatings prepared in example 2 and comparative example 2;
FIG. 3 is a graph of corrosion resistance for composite coatings prepared in example 3 and comparative example 3;
FIG. 4 is a graph of corrosion resistance of composite coatings prepared in comparative example 4 and comparative example 5;
fig. 5 is a schematic diagram of a wear-resistant and corrosion-resistant mechanism of the bottom surface integrated composite coating provided by the invention.
Detailed Description
The invention provides a bottom surface integrated composite coating, which comprises an A component and a B component which are independently subpackaged;
the component A is prepared from 0-5% of modified graphene, 50-70% of fluorocarbon resin, 4-10% of epoxy resin, 0-30% of titanium dioxide, 0.2-1.0% of dispersing agent, 0.6-1.8% of organic soil, 10-20% of organic solvent, 0.2-0.5% of defoaming agent and 0-0.4% of flatting agent by mass percentage; the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene;
the component B is an isocyanate curing agent;
the mass ratio of the component A to the component B is 100:10 to 20.
The bottom surface integrated composite coating provided by the invention comprises a component A. The component A is prepared from 0-5% of modified graphene, preferably 0.05-2% of modified graphene. In the invention, the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene.
In the present invention, the preparation method of fluorinated graphene preferably includes: mixing graphite Fluoride (FGi) with an ethanol solution containing a stabilizer, and performing ultrasonic dispersion to obtain a graphite fluoride dispersion liquid; and shearing and stripping the graphite fluoride dispersion liquid at a high speed to obtain Fluorinated Graphene (FG). In the present invention, the fluorine content of the graphite fluoride is preferably 50 to 65 atom%. In the present invention, the stabilizer is preferably polyvinylpyrrolidone (PVP); the concentration of the stabilizer in the ethanol solution containing the stabilizer is preferably 5-15 mg/mL. In the present invention, the concentration of graphite fluoride in the graphite fluoride dispersion liquid is preferably 0.4 to 3.2mg/mL, more preferably 0.6 to 2.4mg/mL, and still more preferably 1.6 mg/mL. In the invention, the time for ultrasonic dispersion is preferably 20-90 min, and more preferably 30-60 min; the ultrasonic power of the ultrasonic dispersion is preferably 100-300W. In the invention, the shearing speed of the high-speed shearing peeling is preferably 5000-20000 r/min, more preferably 6000-16000 r/min, and further preferably 12000 r/min; the time for the high-speed shearing and stripping is preferably 5-15 h, more preferably 7-13 h, and further preferably 10 h. The present invention preferably further comprises, after the high shear peeling: centrifuging the obtained system to obtain a supernatant; carrying out suction filtration on the supernatant to obtain a solid substance; and drying the solid matter to obtain the fluorinated graphene. In the invention, the rotation speed of the centrifugal treatment is preferably 2000-5000 r/min, and more preferably 3000-4000 r/min; the time of the centrifugal treatment is preferably 5-15 min. The invention removes the excessive stabilizer by suction filtration. In the invention, the drying temperature is preferably 60 ℃, and the drying time is preferably 12 hours; the drying is preferably vacuum drying.
In the invention, the mass ratio of the fluorinated graphene to the zirconium phosphate in the zirconium phosphate modified fluorinated graphene is preferably 0.5-1: 0.25 to 2.
In the present invention, the preparation method of the zirconium phosphate modified fluorinated graphene preferably includes: mixing FG, Dopamine (DA), zirconium phosphate (ZrP) and Tris buffer solution to obtain a mixed solution; and carrying out solid-liquid separation on the mixed solution, and drying the obtained solid to obtain the zirconium phosphate modified fluorinated graphene. In the present invention, the zirconium phosphate is preferably α -zirconium phosphate (α -ZrP). In the present invention, the FG, DA, and ZrP mass ratio is preferably 1: 0.5-1: 2; the concentration of DA in the mixed solution is preferably 0.5-4 mg/mL. In the present invention, the Tris buffer solution preferably has a pH of 8.5 and a concentration of 10 mmol/L. In the present invention, the FG, DA, ZrP and Tris buffer solution mixing preferably comprises: FG, DA, ZrP were dissolved in Tris buffer solution, respectively, and mixed. In the present invention, the temperature of the mixing is preferably 25 ℃; the mixing is preferably carried out under stirring conditions; the stirring speed is preferably 100-400 r/min; the stirring time is preferably 12-24 h. In the present invention, the method of solid-liquid separation is preferably centrifugation; the rotating speed of the centrifugation is preferably 8000-12000 r/min. In the centrifugal process, deionized water is preferably adopted for washing until the pH value of the upper layer solution is 7; the number of times of washing with deionized water is preferably 3 to 7 times, and more preferably 4 to 6 times. In the invention, the drying temperature is preferably 60 ℃, and the drying time is preferably 12 hours; the drying is preferably vacuum drying. In the present invention, DA is self-polymerized in an aqueous solution, and then a PDA layer is formed on the surface of the material. According to the invention, PDA is used as an interlayer adhesive, and the layered zirconium phosphate (alpha-ZrP) can be assembled on the surface of the Fluorinated Graphene (FG) by modifying the fluorinated graphene by using zirconium phosphate.
The component A is prepared from 50-70% by mass of fluorocarbon resin, preferably 50-60% by mass of fluorocarbon resin. In the invention, the fluorocarbon resin is preferably hydroxyl FEVE resin, and the hydroxyl value is preferably 40-100 mg KOH/g.
The component A is prepared from 4-10% by mass of epoxy resin, and preferably 5-8% by mass of epoxy resin. In the present invention, the epoxy resin is preferably E51. In the invention, the mass ratio of the fluorocarbon resin to the epoxy resin is preferably 95-70: 5-30, more preferably 90-80: 10 to 20.
The preparation raw material of the component A comprises 0-30% by mass of titanium dioxide, and preferably 25% by mass of titanium dioxide.
The component A is prepared from 0.2-1.0% of a dispersing agent by mass percentage, and preferably 0.5% of the dispersing agent by mass percentage. In the present invention, the dispersant is preferably an acrylic copolymer ammonium salt and/or an acrylic copolymer sodium salt.
The component A is prepared from 0.6-1.8% of organic soil by mass percent, and preferably 1.0% of organic soil by mass percent. In the present invention, the organic soil is preferably bentonite.
The component A is prepared from 10-20% by mass of an organic solvent, and preferably 12-16% by mass of the organic solvent. In the present invention, the organic solvent preferably includes one or more of ethanol, acetone, xylene, and butyl acetate.
The component A is prepared from 0.2-0.5% of defoaming agent, preferably 0.3-0.4% of defoaming agent. In the present invention, the defoaming agent is preferably a polyether-modified silicone-based defoaming agent.
The component A is prepared from 0-0.4% of a leveling agent, preferably 0.1-0.3% of a leveling agent. In the present invention, the leveling agent is preferably a modified silicone leveling agent.
The bottom surface integrated composite coating provided by the invention comprises a component B. In the present invention, the B component is an isocyanate-based curing agent, and more preferably an HDI trimer or HDI biuret.
In the invention, the mass ratio of the component A to the component B is 100:10 to 20.
The invention provides a preparation method of the integrative composite coating of the bottom surface in the technical scheme, which comprises the following steps:
mixing the preparation raw materials of the component A to obtain a component A;
and mixing the component A and the component B to obtain the bottom surface integrated composite coating.
The preparation method of the component A is explained in detail, and the preparation raw materials of the component A are mixed to obtain the component A. In the present invention, the mixing is preferably performed at room temperature, and more preferably at 25 to 40 ℃. In the present invention, the preparation raw material mixing of the a component preferably includes: carrying out first mixing on modified graphene and an organic solvent to obtain a modified graphene dispersion liquid; carrying out second mixing on the modified graphene dispersion liquid and epoxy resin to obtain epoxy resin dispersion liquid; thirdly mixing the epoxy resin dispersion liquid and fluorocarbon resin to obtain composite resin dispersion liquid; and fourthly mixing the composite resin dispersion liquid, titanium dioxide, a dispersing agent, organic soil, a defoaming agent and a flatting agent to obtain the component A.
According to the invention, the modified graphene and the organic solvent are preferably subjected to first mixing to obtain the modified graphene dispersion liquid. In the present invention, the first mixing is preferably ultrasonic mixing; the power of ultrasonic mixing is preferably 100-300W, and more preferably 200W; the time for the first mixing is preferably 10 to 60min, and more preferably 30 to 50 min.
After the modified graphene dispersion liquid is obtained, the modified graphene dispersion liquid and the epoxy resin are preferably subjected to second mixing to obtain the epoxy resin dispersion liquid. In the present invention, the second mixing is preferably ultrasonic plus mechanical stirring; the power of the ultrasonic wave is preferably 80-200W; the rotating speed of the mechanical stirring is preferably 200-1000 r/min; the time of the second mixing is preferably 5-20 min.
After the epoxy resin dispersion liquid is obtained, the epoxy resin dispersion liquid and the fluorocarbon resin are preferably subjected to third mixing to obtain the composite resin dispersion liquid. In the present invention, the third mixing is preferably mechanical stirring; the rotating speed of the mechanical stirring is preferably 200-1000 r/min; the time for the third mixing is preferably 1 to 4 hours, and more preferably 2 to 3 hours. In the present invention, the temperature of the third mixing is preferably 25 to 40 ℃.
After the composite resin dispersion liquid is obtained, the composite resin dispersion liquid, titanium dioxide, a dispersing agent, organic soil, a defoaming agent and a leveling agent are preferably subjected to fourth mixing to obtain the component A. In the present invention, the feeding sequence of the fourth mixing is preferably to sequentially add titanium dioxide, dispersant, organic soil, defoamer and leveling agent into the composite resin dispersion. In the invention, the fourth mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 1000-2000 r/min; the time for the fourth mixing is preferably 30-60 min.
After the component A is prepared, the component A and the component B are mixed to obtain the bottom surface integrated composite coating. In the present invention, the mixing is preferably mechanical stirring; the rotating speed of the mechanical stirring is preferably 200-300 r/min; the mixing time is preferably 30-90 min, and more preferably 60 min. In the present invention, the mixing temperature is preferably 25 to 40 ℃.
The invention provides a coating method of a bottom surface integrated composite coating, which comprises the steps of coating the bottom surface integrated composite coating or the bottom surface integrated composite coating prepared by the preparation method of the technical scheme on the surface of a substrate in one step, and curing at room temperature to obtain the composite coating. In the present invention, the substrate preferably includes a metal substrate, a building substrate, or a wood substrate. In the present invention, the metal substrate is preferably tinplate. In the invention, before the coating, the metal substrate is preferably pretreated; the pre-treatment of the metal substrate preferably comprises sanding, washing and drying in sequence. In the invention, the sand paper polishing preferably sequentially adopts 400-mesh, 800-mesh and 1200-mesh sand paper to polish the metal substrate; the cleaning is preferably acetone or ethanol.
In the present invention, the one-step coating means preferably includes blade coating, spin coating or spray coating. In the invention, the room temperature curing time is preferably 8-36 h, and more preferably 12-24 h.
The bottom surface integrated composite coating is prepared by blending the epoxy resin which is low in cost, has unique physical and chemical properties and good adhesion to a substrate and the fluorocarbon resin which is low in surface energy and excellent in wear-resistant and corrosion-resistant effects, and the wear-resistant and corrosion-resistant properties of the bottom surface integrated composite coating are enhanced by further introducing the fluorinated graphene which is excellent in lubricating ability, high in bearing ability and excellent in wear resistance and has a lamellar structure. The invention can obtain high-efficiency protective coating on the surface of the substrate, and prolong the service life of metal substrate materials such as ship parts, ocean facilities and the like under complex working conditions.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Preparing fluorinated graphene: FGi is added into ethanol solution containing 10mg/mL PVP to prepare dispersion liquid with the concentration of graphite fluoride of 1.6 mg/mL; performing ultrasonic dispersion for 30min by using 100W ultrasonic equipment, transferring the prepared dispersion liquid into a special high-speed stirring container, and stirring for 10h in a high-speed shearing machine with the rotating speed of 12000r/min to obtain a black mixed solution; then centrifuging the mixed solution at 3000r/min for 15min, and taking supernatant; and (4) leaching to remove excessive PVP, and finally drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain Fluorinated Graphene (FG) powder.
Uniformly dispersing fluorinated graphene and xylene through ultrasonic treatment, wherein the ultrasonic power is 200W, and the ultrasonic time is 30min, so as to obtain a fluorinated graphene dispersion liquid with the concentration of 3 mg/mL; adding epoxy resin, stirring to obtain a uniform mixed solution, adding fluorocarbon resin, mechanically stirring for 3 hours, and then sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent to obtain a component A; the component A comprises the following raw materials in percentage by mass: 0.5% of fluorinated graphene, 6.3% of epoxy resin, 56.5% of fluorocarbon resin, 25% of titanium dioxide, 0.5% of dispersing agent, 1.0% of organic soil, 10% of organic solvent and 0.2% of defoaming agent;
and stirring and mixing the component A and the component B HDI tripolymer for 60min at the rotating speed of 200r/min according to the mass ratio of 100:10 to obtain the bottom surface integrated composite coating.
Grinding by using 400-mesh, 800-mesh and 1200-mesh sand paper in sequence by taking tinplate as a substrate, wiping by using acetone and drying; uniformly coating the bottom surface integrated composite coating on the tinplate in one step by adopting a blade coating method, wherein the coating thickness is 100 +/-10 mu m, and drying at room temperature for 48h to obtain the composite coating.
Comparative example 1
Uniformly dispersing reduced graphene oxide and xylene through ultrasonic treatment, wherein the ultrasonic power is 2000W, and the ultrasonic time is 30min, so as to obtain a graphene oxide dispersion liquid with the concentration of 3 mg/mL; adding epoxy resin, stirring to obtain a uniform mixed solution, adding fluorocarbon resin, mechanically stirring for 3h, sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 0.5% of graphene oxide, 6.3% of epoxy resin, 56.5% of fluorocarbon resin, 25% of titanium dioxide, 0.5% of dispersing agent, 1.0% of organic soil, 10% of organic solvent and 0.2% of defoaming agent;
and stirring and mixing the component A and the component B HDI trimer at the rotating speed of 200r/min for 60min according to the mass ratio of 100:10 to obtain the composite coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; and uniformly coating the composite coating on the tinplate by a blade coating method in one step, wherein the coating thickness is 100 +/-10 mu m, and drying at room temperature for 48 hours to prepare the composite coating.
Example 2
FG, DA, ZrP were dissolved in Tris buffer solution (pH 8.5, 10mmol/L) respectively, with DA concentration of 2mg/mL, FG, DA, α -ZrP mass ratio of 1: 1: and 2, stirring for 24 hours at 25 ℃, wherein the stirring speed is 200r/min, centrifuging after obtaining a mixed solution, washing for 4 times by using deionized water until the pH value of the upper-layer solution is 7 to obtain a lower-layer precipitate, and drying for 12 hours in a vacuum drying oven at 60 ℃ to obtain the zirconium phosphate modified fluorinated graphene.
Uniformly dispersing zirconium phosphate modified fluorinated graphene and xylene through ultrasonic treatment, wherein the ultrasonic power is 80W, and the ultrasonic time is 10min, so as to obtain a zirconium phosphate modified fluorinated graphene dispersion liquid with the concentration of 2 mg/mL; adding epoxy resin, stirring to obtain a uniform mixed solution, adding fluorocarbon resin, mechanically stirring for 3h, sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 0.5% of zirconium phosphate modified fluorinated graphene, 6.3% of epoxy resin, 56.5% of fluorocarbon resin, 25% of titanium dioxide, 0.5% of dispersing agent, 1.0% of organic soil, 10% of organic solvent and 0.2% of defoaming agent;
and stirring and mixing the component A and the component B HDI tripolymer for 30min at the rotating speed of 300r/min according to the mass ratio of 100:10 to obtain the bottom surface integrated composite coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; uniformly coating the bottom surface integrated composite coating on a tinplate in one step by adopting a blade coating method, wherein the coating thickness is 100 +/-10 mu m, and drying at room temperature for 72h to obtain the composite coating.
Comparative example 2
Uniformly dispersing zirconium phosphate and xylene through ultrasonic treatment, wherein the ultrasonic power is 80W, and the ultrasonic time is 10min, so as to obtain a zirconium phosphate dispersion liquid with the concentration of 2 mg/mL; adding epoxy resin, stirring to obtain a uniform mixed solution, adding fluorocarbon resin, mechanically stirring for 3h, sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 0.5 percent of zirconium phosphate, 6.3 percent of epoxy resin, 56.5 percent of fluorocarbon resin, 25 percent of titanium dioxide, 0.5 percent of dispersant, 1.0 percent of organic soil, 10 percent of organic solvent and 0.2 percent of defoaming agent;
and stirring and mixing the component A and the component B HDI tripolymer for 30min at the rotating speed of 300r/min according to the mass ratio of 100:10 to obtain the composite coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; uniformly coating the composite coating on a tinplate in one step by adopting a blade coating method, wherein the coating thickness is 100 +/-10 mu m, and drying at room temperature for 72h to obtain the composite coating.
Example 3
Mixing epoxy resin and acetone, and performing ultrasonic treatment for 20min until the mixture is uniformly dispersed to obtain an epoxy resin solution; adding fluorocarbon resin into the epoxy resin solution, stirring at a stirring speed of 300r/min until the fluorocarbon resin is uniform, then sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 6.3 percent of epoxy resin, 57.0 percent of fluorocarbon resin, 25 percent of titanium dioxide, 0.5 percent of dispersant, 1.0 percent of organic soil, 10 percent of organic solvent and 0.2 percent of defoaming agent;
and uniformly mixing the component A and the component B HDI trimer according to the mass ratio of 100:10 to obtain the bottom surface integrated composite coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; and uniformly coating the bottom surface integrated composite coating on the tinplate in one step by adopting blade coating, wherein the coating thickness is 100 +/-10 mu m, and drying for 24 hours at room temperature to prepare the composite coating.
Comparative example 3
Mixing dimethylbenzene and fluorocarbon resin, stirring at a stirring speed of 220r/min until the mixture is uniform, then sequentially adding titanium dioxide, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 63.3 percent of fluorocarbon resin, 25 percent of titanium dioxide, 0.5 percent of dispersant, 1.0 percent of organic soil, 10 percent of organic solvent and 0.2 percent of defoaming agent;
and uniformly mixing the component A and the component B HDI trimer according to the mass ratio of 100:10 to obtain the fluorocarbon coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; uniformly coating the fluorocarbon coating on the tinplate in one step by adopting a blade coating method, wherein the coating thickness is 100 +/-10 mu m, and drying for 24h at room temperature to obtain the composite coating.
Comparative example 4
Dissolving pure epoxy resin in acetone, stirring at a stirring speed of 220r/min until the mixture is uniform, then sequentially adding talcum powder, a dispersing agent, organic soil and a defoaming agent, and stirring for 30min to obtain a component A; the component A comprises the following raw materials in percentage by mass: 63.3 percent of epoxy resin, 25 percent of talcum powder, 0.5 percent of dispersant, 1.0 percent of organic soil, 10 percent of organic solvent and 0.2 percent of defoaming agent; obtaining a component A; and the component B is a polyether amine (D400) curing agent, and the component A and the component B are uniformly mixed according to the mass ratio of 100:10 to obtain the epoxy coating.
Grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; uniformly coating the epoxy coating on the tinplate in one step by adopting a blade coating method, wherein the coating thickness is 100 +/-10 mu m, and curing for 45min at 90 ℃ and 3h at 135 ℃ in sequence to prepare the epoxy coating.
Comparative example 5
Preparing fluorocarbon paint and epoxy paint according to comparative example 3 and comparative example 4 respectively;
grinding tinplate serving as a substrate by sequentially adopting 400-mesh, 800-mesh and 1200-mesh sand paper, wiping by using acetone, and drying; the epoxy-fluorocarbon double-layer coating is prepared by two steps by adopting a blade coating method and taking epoxy coating as primer (the coating thickness is 50 +/-5 mu m) and fluorocarbon coating as finish (the coating thickness is 50 +/-5 mu m).
Test example
Table 1 shows the mechanical properties and the friction coefficients and the wear rates of the composite coatings prepared in examples 1 to 3 and comparative examples 1 to 5 under different friction conditions. Comparing various data of mechanical properties, it can be seen that the fluorocarbon coating added with the solid lubricant (fluorinated graphene or zirconium phosphate modified fluorinated graphene) has excellent mechanical properties, and comparing the friction coefficient and the wear rate, it can be seen that the friction coefficient and the wear rate of the fluorocarbon coating modified by the fluorinated graphene and the zirconium phosphate modified fluorinated graphene are lower than those of the fluorocarbon coating prepared by the comparative example, which indicates that the fluorinated graphene can more effectively improve the friction and wear properties of the fluorocarbon coating. Meanwhile, the fluorinated graphene and the zirconium phosphate modified fluorinated graphene contain a large number of C-F bonds which are the same as those of the fluorocarbon coating, so that the wear-resistant and corrosion-resistant properties of the composite coating can be obviously improved. The data in the table 1 are combined to show that the bottom surface integrated composite coating provided by the invention can obtain a fluorocarbon composite coating with excellent mechanical property, friction and corrosion performance, and has good application prospect in the fields of materials, machinery and the like.
Fig. 1 to 4 are corrosion impedance diagrams of the composite coatings prepared in examples 1 to 3 and comparative examples 1 to 5, respectively, and comparing the impedance arc radii of the coatings, it can be found that the impedance arc of the fluorocarbon coating modified by the fluorinated graphene and the zirconium phosphate modified fluorinated graphene is larger than that of the comparative example, which indicates that the coating has the best protection performance on the metal substrate and has excellent corrosion resistance.
The wear-resistant and corrosion-resistant mechanism is analyzed by combining with fig. 5, the modified fluorinated graphene contains a rigid carbon atom network structure, the excellent mechanical property of the modified fluorinated graphene can improve the friction stress resistance of the coating, and meanwhile, the modified fluorinated graphene has a lamellar structure, so that the diffusion path of a corrosive medium can be effectively blocked, the permeation path of the corrosive substance becomes tortuous to form a labyrinth effect, and the wear-resistant and corrosion-resistant performance of the coating is effectively improved.
TABLE 1 mechanical properties and friction coefficients and wear rates under different friction conditions of the composite coatings prepared in examples 1-3 and comparative examples 1-5
Note: the friction coefficient and the wear rate are measured by a sample on a CFT-I type material surface comprehensive performance tester, and the test conditions are as follows: normal temperature, 3N, 300r/min, friction conditions: dry rub and simulated seawater (3.5 wt% NaCl solution) rub conditions.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A bottom surface integrated composite coating comprises an A component and a B component which are independently packaged;
the component A is prepared from 0-5% of modified graphene, 50-70% of fluorocarbon resin, 4-10% of epoxy resin, 0-30% of titanium dioxide, 0.2-1.0% of dispersing agent, 0.6-1.8% of organic soil, 10-20% of organic solvent, 0.2-0.5% of defoaming agent and 0-0.4% of flatting agent by mass percentage; the modified graphene is fluorinated graphene or zirconium phosphate modified fluorinated graphene;
the component B is an isocyanate curing agent;
the mass ratio of the component A to the component B is 100:10 to 20.
2. The primer-topcoat integrated composite coating of claim 1, wherein the fluorocarbon resin is a hydroxyl FEVE resin, and the hydroxyl value is 40-100 mg KOH/g; the mass ratio of the fluorocarbon resin to the epoxy resin is 95-70: 5 to 30.
3. The primer-topcoat integrated composite coating of claim 1, wherein the preparation method of the fluorinated graphene comprises: mixing graphite fluoride and an ethanol solution containing a stabilizer, and performing ultrasonic dispersion to obtain a graphite fluoride dispersion liquid; and shearing and stripping the graphite fluoride dispersion liquid at a high speed to obtain the fluorinated graphene.
4. The primer-integrated composite coating of claim 3, wherein the stabilizer is polyvinylpyrrolidone; the concentration of the stabilizer in the ethanol solution containing the stabilizer is 5-15 mg/mL; the shearing speed of the high-speed shearing stripping is 5000-20000 r/min, and the time is 5-15 h; the concentration of the graphite fluoride in the graphite fluoride dispersion liquid is 0.4-3.2 mg/mL.
5. The primer-topcoat integrated composite coating as claimed in claim 1, wherein the mass ratio of the fluorinated graphene to the zirconium phosphate in the zirconium phosphate modified fluorinated graphene is 0.5-1: 0.25 to 2.
6. The primer-topcoat integrated composite coating of claim 1 or 5, wherein the preparation method of the zirconium phosphate modified fluorinated graphene comprises: mixing fluorinated graphene, dopamine and a Tris buffer solution to obtain a mixed solution; and carrying out solid-liquid separation on the mixed solution, and drying the obtained solid to obtain the zirconium phosphate modified fluorinated graphene.
7. The preparation method of the integral bottom composite coating of any one of claims 1 to 6, comprising the following steps:
mixing the preparation raw materials of the component A to obtain a component A;
when in use, the component A and the component B are mixed to obtain the bottom surface integrated composite coating.
8. The preparation method according to claim 7, wherein the raw material mixture for preparing the A component comprises:
carrying out first mixing on modified graphene and an organic solvent to obtain a modified graphene dispersion liquid;
carrying out second mixing on the modified graphene dispersion liquid and epoxy resin to obtain epoxy resin dispersion liquid;
thirdly mixing the epoxy resin dispersion liquid and fluorocarbon resin to obtain composite resin dispersion liquid;
and fourthly mixing the composite resin dispersion liquid, titanium dioxide, a dispersing agent, organic soil, a defoaming agent and a flatting agent to obtain the component A.
9. A coating method of the bottom surface integrated composite coating is characterized in that the bottom surface integrated composite coating as described in any one of claims 1 to 6 or the bottom surface integrated composite coating prepared by the preparation method as described in any one of claims 7 to 8 is coated on the surface of a substrate in one step and cured at room temperature to obtain the composite coating.
10. The coating method according to claim 9, wherein the one-step coating manner comprises blade coating, spin coating or spray coating; the room temperature curing time is 8-36 h.
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| CN116121573B (en) * | 2023-03-14 | 2024-01-02 | 创拓精工(江苏)有限公司 | Nut with composite coating on surface and preparation method thereof |
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Application publication date: 20220830 |