CN112745723A - Water-based fluorocarbon resin heavy-duty anticorrosive paint and preparation method thereof - Google Patents
Water-based fluorocarbon resin heavy-duty anticorrosive paint and preparation method 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
- 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
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- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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- 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
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- 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
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- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a water-based fluorocarbon resin heavy-duty anticorrosive paint and a preparation method thereof. The anticorrosive paint comprises the following components in mass: 50-60% of water-based fluorocarbon resin, 8-15% of water, 2-3% of dispersing agent, 0.1-1.0% of defoaming agent, 0.6-1.0% of thickening agent, 18-28% of titanium dioxide, 1-4% of film-forming assistant, 4-9% of curing agent, 0.1-3% of wetting dispersing agent and 0.1-3% of modified graphene or graphene-carbon nanotube; the modified graphene or graphene-carbon nanotube is polymer-coated graphene or graphene/carbon nanotube. The modified graphene or graphene/carbon nano tube added in the coating disclosed by the invention is coated with the polymer, so that the solubility is improved, and the mechanical strength, hardness and adhesiveness of the fluorocarbon coating can be greatly improved. The fluorocarbon coating disclosed by the invention takes water as a solvent, meets the anticorrosive requirement and has the characteristics of cleanness and environmental protection.
Description
Technical Field
The invention relates to a water-based fluorocarbon coating, in particular to a water-based fluorocarbon resin heavy-duty anticorrosive coating added with modified graphene and graphene/carbon nano tubes.
Background
Corrosion is the process of damaging metal, concrete, wood and other substrates by physical, chemical or electrochemical action. Each year, economic losses due to corrosion are enormous and potential safety hazards are set in burial for their use at a later date. Therefore, the research on preservation has been increasingly paid attention. Among the various means of corrosion protection, anticorrosive coatings are the most economical, convenient and safe method.
The water-based fluorocarbon resin is a vinyl fluoride-alkyl vinyl ether/ester alternating copolymer which can be cured at normal temperature, the water solubility, the good adhesion, the compatibility with the filler and other properties of the resin are endowed by introducing different alkyl vinyl ethers/esters, and meanwhile, the vinyl fluoride monomer can well protect the main chain, so that the resin has excellent aging resistance, weather resistance and chemical stability, and is a coating resin matrix with great potential and wide prospect.
In recent years, due to the unique physicochemical properties of carbon materials, the mechanical property, compactness and corrosion resistance of the coating can be effectively improved by adding a small amount of carbon materials. Meanwhile, due to the characteristics of the graphene and the carbon nano tube, the coating can be endowed with special properties such as electric conduction and heat conduction, wave absorption, self-cleaning and the like. Therefore, graphene and carbon nanotubes have become hot spots for the research on the functional filler of the anticorrosive paint.
When two materials with chemical properties of conductivity (static electricity) and potential are contacted, a corrosion couple is formed due to the existence of potential difference. The galvanic series of the carbon steel is-0.40, so that all materials with the potential higher than-0.40 are in contact with the carbon steel to form a corrosion galvanic couple with the carbon steel, thereby causing the corrosion of the carbon steel. It is known that the carbon material coating has a galvanic series potential of 0.20-0.30, and when such a coating is applied, water, oxygen or other ions penetrate into the interface between the carbon steel and the coating once the coating is broken, thereby accelerating the corrosion of the carbon steel. The carbon material must therefore be modified in order to protect the carbon steel.
The polymer is adopted to coat the graphene and the carbon nano tube, a large number of functional groups are introduced while the complete tubular structure of the graphene and the carbon nano tube is maintained, the excellent mechanical properties of the graphene and the carbon nano tube are maintained, the dispersity and the compatibility with a film forming substance of the graphene and the carbon nano tube are improved, the direct contact between carbon materials and the coating is avoided, the conductivity of the coating is reduced, and the risk of galvanic corrosion with steel is avoided. Thereby improving the strength of the fluorocarbon coating, improving the hardness of the fluorocarbon coating, having higher adhesiveness and good heavy corrosion resistance.
Under severe circumstances, the polymer is adopted to coat the carbon nano tube, and the prepared coating has good adhesive force, but has poor dispersion effect and poor mechanical property. The modified graphene and the synergetic modified graphene/carbon nano tube are adopted to improve the dispersibility and the mechanical property of the coating.
CN110066556A discloses a modified graphene reinforced aqueous FEVE fluorocarbon flexible protective coating, which comprises the following components: the modified graphene functional material comprises water-based FEVE fluorocarbon resin, a low surface energy auxiliary agent, a curing agent, a diluent and a grafted modified graphene functional filler. According to the invention, the silane coupling agent gamma-aminopropyl triethylsilane is used for grafting modification of graphene, so that the wettability of the graphene is effectively improved, and the graphene is uniformly dispersed in a coating system; the grafted modified graphene with the sheet structure is uniformly dispersed, stacked layer by layer and staggered in the aqueous FEVE fluorocarbon resin to form a tight physical shielding structure, water molecules and atmospheric corrosion media are effectively prevented from permeating or diffusing into a circuit board matrix, and the excellent low surface energy and hydrophobic characteristics of the fluororesin are combined, so that the prepared protective coating has the functions of water resistance, moisture resistance and salt mist corrosion resistance, and has good reliability under the extreme working conditions of high temperature, high humidity and high salt mist corrosion.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a water-based fluorocarbon resin heavy-duty anticorrosive coating in a first aspect.
The specific technical scheme is as follows:
the water-based fluorocarbon resin heavy-duty anticorrosive paint comprises the following components in parts by mass:
50-60 wt% of water-based fluorocarbon resin, 8-15 wt% of water, 2-3% of dispersing agent, 0.1-1.0% of defoaming agent, 0.6-1.0% of thickening agent, 18-28% of titanium dioxide, 1-4% of film forming additive, 4-9% of curing agent, 0.1-3% of wetting dispersing agent, 0.1-3% of modified graphene or graphene-carbon nano tube, wherein the modified graphene or graphene-carbon nano tube is polymer-coated graphene or graphene/carbon nano tube.
Further, the content of the wetting dispersant is 0.1% -2%.
The polymer is polyvinyl acetate or vinyl acetate/vinyl versatate copolymer. The content of the polymer in the modified graphene or graphene/carbon nanotube is generally 1wt% -20 wt%.
The dispersant is conventional dispersant in the field, such as one or more selected from BYK-162, BYK-192, BYK-190, BYK-9076, BYK-111, BYK-AT204 and BYK-110.
The defoaming agent is selected from one or more of BYK-A555, BYK-022, BYK-052, BYK-088, BYK-011, BYK-019 and BYK-065.
The thickening agent is one selected from BYK-420, BYK-425, UH-420, BYK-428, BYK-410 and BYK-A200.
The film-forming assistant and the curing agent are all conventional materials in the field. The film forming auxiliary agent can be one or more selected from propylene glycol butyl ether, alcohol ester twelve and methyl glycol methyl ether acetate. The curing agent may be at least one selected from the group consisting of Nippon 4F curing agents.
The wetting dispersant is one or more of BYK-163, BYK-P104, BYK-9077, BYK-Au203 and BYK-168.
The modified graphene or the modified graphene/carbon nanotube adopts the following preparation method:
firstly, dissolving a surfactant in an acetic acid/sodium acetate buffer solution with the pH value of 3-5 to prepare a solution with the concentration of 3 multiplied by 10-3~6×10-3A surfactant solution in mol/L;
dispersing a proper amount of graphene or graphene/carbon nano tubes in a surfactant solution to obtain an emulsion;
adding monomer vinyl acetate or vinyl acetate/vinyl versatate (PVAc/V10) into the emulsion obtained in the step (c);
adding ammonium persulfate into the emulsion obtained in the step (III), wherein the mass of the ammonium persulfate is 15-35 wt% of the content of monomer vinyl acetate or vinyl acetate/vinyl versatate, heating and reacting;
demulsifying by using a magnesium sulfate solution, filtering, washing, and drying to obtain the polymer-coated modified graphene or graphene/carbon nanotubes.
Further, in the preparation method of the modified graphene or the modified graphene/carbon nanotube, the step (i) further comprises the operation of carrying out reduced pressure distillation and purification on monomer vinyl acetate and vinyl versatate.
In the second step, before dissolving in the surfactant solution, the graphene or graphene/carbon nanotubes are preferably ground, and more preferably ball-milled in a planetary ball mill. After dispersing in the surfactant solution, preferably performing ultrasonic dispersion for 30-80 min to promote mixing.
In the third step, when vinyl acetate-vinyl versatate are added, the mass fraction of the vinyl acetate is 70wt% -90 wt%, and the mass fraction of the vinyl versatate is 10wt% -30 wt%. The mass ratio of the graphene or the graphene/the carbon nano tube to the monomer vinyl acetate or the vinyl acetate/the vinyl versatate is (0-2): (8-10); the molar mass ratio of the total molar mass of the monomers to the surfactant is (0-3): (8-12). And step three, adding the monomer and stirring at a high speed.
The mass concentration of the magnesium sulfate solution is generally 30-40 g/L.
The surfactant can be selected from KH550 or OP-10 or sodium dodecyl benzene sulfonate or Tween-80.
The carbon nanotube of the present invention includes a single-walled carbon nanotube and a multi-walled carbon nanotube.
The invention also provides a preparation method of the heavy-duty anticorrosive paint. The preparation method comprises the following steps:
(1) adding water, a dispersing agent, a defoaming agent and a thickening agent according to a proportion, and uniformly mixing to obtain an A1 component; adding titanium dioxide, and continuously and uniformly mixing to obtain a component A;
(2) uniformly mixing the water-based fluorocarbon resin and the defoaming agent to obtain a component B; adding the component B into the component A, adding the film-forming assistant, and uniformly mixing;
(3) dispersing the modified graphene or graphene/carbon nano tube and the wetting dispersant to obtain a component C; and (3) adding the component C into the system obtained in the step (2), uniformly mixing, adding a curing agent, and uniformly mixing to obtain the heavy anti-corrosion coating.
Further, the preparation method of the modified graphene or graphene/carbon nanotube is as described above.
Wherein the dispersant is one or more of BYK-162, BYK-192, BYK-190, BYK-9076, BYK-111, BYK-AT204 and BYK-110.
The defoaming agent is one or more of BYK-A555, BYK-022, BYK-052, BYK-088, BYK-011, BYK-019 and BYK-065.
The thickener is one of BYK-420, BYK-425, UH-420, BYK-428, BYK-410 and BYK-A200.
The defoaming agent is one or more of BYK-141, BYK-1710, BYK-021, BYK-A501 and BYK-054.
The wetting dispersant is one or more of BYK-163, BYK-P104, BYK-9077, BYK-Au203 and BYK-168.
In the step (1), firstly, mixing the components in A1, mechanically stirring for 10-45 min, and rotating at 500-1000 r/min; then adding A2 titanium dioxide, and mechanically stirring for 90-180 min at a rotation speed of 600-1000 r/min.
In the step (2), the component B is prepared, and the aqueous fluorocarbon resin and the defoaming agent are mixed for 15-45 min. And pouring the component B into the component A, and adding a film-forming aid (wherein the film-forming agent is one or more of propylene glycol butyl ether, alcohol ester dodeca and methyl glycol monomethyl ether acetate).
In the step (3), the component C is prepared, a dispersion solution is prepared by using a wetting dispersant, the modified graphene or graphene/carbon nano tube is subjected to ball milling in a planetary ball mill for 10-30 min and then subjected to ultrasonic dispersion for 15-45 min, and the component C dispersion solution is obtained.
The A, B, C components are mixed and stirred evenly by a machine, the stirring time is 45-150 min, and the rotating speed is 500-1000 r/min. And adding a Nippon 4F curing agent into the mixed solution, and magnetically stirring for 15-45 min to prepare the heavy-duty anticorrosive paint.
Preferably, the coating is sprayed using a spray gun.
Compared with the prior art, the invention has the advantages that:
1. the fluorocarbon coating is widely applied to the field of heavy corrosion protection due to excellent weather resistance, solvent resistance and chemical resistance. Since the 21 st century, due to the increasing awareness of environmental protection, the pursuit of coatings is not limited to excellent functionality (corrosion resistance, heat insulation, wear resistance, etc.), and restrictions on VOCs are becoming more stringent. The research and development of water-based, high-solid and powder coatings instead of traditional solvent coatings is a key point. The water-based fluorocarbon coating uses water as a solvent, maintains excellent aging resistance, weather resistance and chemical stability of the solvent-based fluorocarbon coating, meets the anticorrosive requirement and has the characteristics of cleanness and environmental protection.
2. The mechanical property of the coating can be effectively improved by adding a small amount of modified graphene or graphene/carbon nano tubes into the coating, and meanwhile, a functional network can be formed in the coating, so that the stress is effectively transferred, and the cohesive force of the coating is improved; the graphene and the carbon nano tube can fill gaps of resin and gaps among pigments and fillers by virtue of small sizes of the graphene and the carbon nano tube, so that the compactness of the coating is improved; the multilayer structure can prolong the path of small molecules entering the coating and enhance the corrosion resistance of the coating.
3. The polymer-coated graphene and graphene/carbon nanotubes can effectively improve the solubility of the polymer-coated graphene and graphene/carbon nanotubes, improve the compatibility of the graphene and graphene/carbon nanotubes with resin, avoid the direct contact of the graphene and graphene/carbon nanotubes with a substrate, and reduce the conductivity of a coating, so that the polymer-coated graphene and graphene/carbon nanotubes are an effective modification method. Due to the fact that vinyl acetate is poor in chemical resistance, in order to prevent modified graphene and graphene/carbon nano tubes from becoming weak points in the coating, vinyl versatate and vinyl acetate are selected for copolymerization, solubility and dispersibility of the graphene and the graphene/carbon nano tubes are improved, conductivity is reduced, and therefore mechanical strength, hardness and adhesiveness of the fluorocarbon coating can be greatly improved. Meanwhile, the graphene and the graphene/carbon nano tube are coated by the polymer, so that the carbon nano tube with higher electric potential of couple sequence is prevented from directly acting on carbon steel after the coating is damaged, and the corrosion resistance of the coating can be improved. Meanwhile, the titanium dioxide with a certain content is added, so that the corrosion resistance and hardness of the paint can be improved, and the paint has certain heat insulation performance. According to the invention, graphene and graphene/carbon nanotubes are used in a composite manner with titanium dioxide through polymer modification, so that the corrosion resistance can be ensured, the strength of the composite coating can be improved, and the composite coating has heat insulation performance.
Detailed Description
The invention provides a water-based fluorocarbon resin heavy-duty anticorrosive coating added with modified graphene and graphene/carbon nanotubes, and the technical scheme in the embodiment of the invention will be clearly and completely described below with reference to the embodiment of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be purchased from chemical companies.
Example 1
(1) Preparing modified graphene:
and carrying out reduced pressure distillation purification on the vinyl acetate. Dissolving KH-550 in acetic acid/sodium acetate buffer solution with pH of 3, and dispersing to obtain a concentration of 4 × 10-3KH-550 solution of mol/L. Taking 1.15 g of graphene, carrying out ball milling in a planetary ball mill for 15 min, dissolving in 40 mL of the solution, and carrying out ultrasonic dispersion for 50 min. 3.44 g of vinyl acetate was added thereto, and the mixture was stirred at high speed for 24 hours. 0.52 g of ammonium persulfate was added to the above solution, and the mixture was heated to 80 ℃ to react for 4 hours. Adding 200 mL of 35g/L magnesium sulfate for demulsification, filtering, washing, and drying at 70 ℃ for 8 h to obtain the polyvinyl acetate coated modified graphene.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 4 g of deionized water is added into a 100 mL three-neck flask, 0.90 g of dispersant BYK-110, 0.06 g of defoamer BYK-019 and 0.15 g of thickener BYK-428 are added dropwise, and mechanical stirring is carried out for 25 min (the rotating speed is 700 r/min).
Preparing a component B: 20 g of waterborne fluorocarbon resin is added into a beaker, 0.10 g of defoaming agent BYK-141 is added dropwise, and magnetons are added for electromagnetic stirring for 40 min.
8g of titanium dioxide is added into the component A, and the mixture is stirred evenly (the mechanical stirring is carried out for 100 min, and the rotating speed is 900 r/min).
Pouring the component B into the component A and continuously stirring; mixing 1.1 g of film-forming aid alcohol ester twelve and 0.15 g of thickener UH-420, adding into the mixed solution of the component A and the component B, and stirring for 60 min (the rotating speed is 600 r/min).
Preparing a component C: 0.05 g of wetting dispersant BYK-Au203 was added to 0.22 g of deionized water, and the mixture was stirred uniformly to prepare a dispersant solution. And (3) taking 0.05 g of modified graphene, carrying out ball milling in a planetary ball mill for 15 min, and carrying out ultrasonic dispersion for 30 min to obtain the modified graphene dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
2.6 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 25 min.
The obtained coating comprises the following components in percentage by weight: 53.51% of waterborne fluorocarbon resin, 11.29% of water, 2.41% of dispersant, 0.13% of wetting dispersant, 0.43% of defoaming agent, 0.80% of thickener, 21.40% of titanium dioxide, 2.94% of film-forming assistant, 6.96% of curing agent and 0.13% of modified graphene.
Spray coating with a spray gun.
Comparative example 1 did not include a process for preparing modified graphene, and unmodified graphene was directly used. Otherwise, the material amount and the preparation process were the same as in example 1, to obtain a heavy duty anticorrosive paint.
Example 2
(1) Preparing modified graphene:
the monomers such as vinyl acetate, vinyl versatate and the like are purified by reduced pressure distillation. OP-10 was dissolved in acetic acid/sodium acetate buffer pH 5 to make a 6X 10 concentration-3mol/L of OP-10. Taking 4.34 g of graphene, carrying out ball milling in a planetary ball mill for 50 min, dissolving in 60 mL of the solution, and carrying out ultrasonic dispersion for 80 min. Then 3.26 g of vinyl acetate and 1.08 g of vinyl acetate are added, and the mixture is stirred at a high speed for 24 hours. 1.00 g of ammonium persulfate was added to the above solution, and the mixture was heated to 80 ℃ to react for 4 hours. Adding 170 mL of 40 g/L magnesium sulfate for demulsification, filtering, washing, and drying at 70 ℃ for 8 h to obtain the modified graphene coated by the vinyl acetate-vinyl versatate copolymer.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 5g of deionized water is added into a 100 mL three-neck flask, 1.10 g of dispersing agent, 0.10 g of defoaming agent BYK-052 and 0.14 g of thickening agent BYK-A200 are added dropwise, and mechanical stirring is carried out for 35 min (the rotating speed is 1000 r/min).
Preparing a component B: 28g of aqueous fluorocarbon resin is added into a beaker, 0.10 g of defoaming agent BYK-021 is added dropwise, and magnetons are added to carry out electromagnetic stirring for 40 min.
9g of titanium dioxide is added into the component A, and the mixture is stirred evenly (mechanically for 140 min, and the rotating speed is 700 r/min).
Pouring the component B into the component A and continuously stirring; 1.0 g of film-forming aid propylene glycol butyl ether and 0.16 g of thickening agent BYK-425 are mixed and added into the mixed liquid of the component A and the component B, and the mixture is stirred for 45 min (the rotating speed is 600 r/min).
Preparing a component C: 0.12 g of wetting dispersant BYK-163 was added to 0.40 g of deionized water, and the mixture was stirred uniformly to prepare a dispersant solution. And (3) carrying out ball milling on 0.08 g of modified graphene in a planetary ball mill for 30 min, and carrying out ultrasonic dispersion for 30 min to obtain the modified graphene dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
2.5 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 45 min.
The coating obtained comprises by weight: 58.70% of water-based fluorocarbon resin, 11.32% of water, 2.30% of dispersing agent, 0.25% of wetting dispersing agent, 0.42% of defoaming agent, 0.63% of thickening agent, 18.87% of titanium dioxide, 2.10% of film-forming assistant, 5.24% of curing agent and 0.17% of modified graphene.
Spray coating with a spray gun.
Comparative example 2
Comparative example 2 did not include a process for preparing modified graphene, and unmodified graphene was directly used. Otherwise, the material amount and preparation process were the same as in example 2, to obtain a heavy duty anticorrosive coating.
Example 3
(1) Preparing modified graphene:
the monomers such as vinyl acetate, vinyl versatate and the like are purified by reduced pressure distillation. Sodium dodecylbenzenesulfonate was dissolved in acetic acid/sodium acetate buffer at pH 4 to prepare a 5X 10 concentration-3mol/L sodium dodecyl benzene sulfonate solution. Taking 1.72 g of graphene, carrying out ball milling in a planetary ball mill for 20 min, dissolving in 50 mL of the solution, and carrying out ultrasonic dispersion for 40 min. Then, 2.76 g of vinyl acetate and 0.68 g of vinyl acetate were added and stirred at a high speed for 24 hours. 0.70 g of ammonium persulfate was added to the above solution, and the mixture was heated to 80 ℃ to react for 4 hours. Adding 180 mL of 30g/L magnesium sulfate for demulsification, filtering, washing, and drying at 70 ℃ for 8 h to obtain the modified graphene coated by the vinyl acetate-vinyl versatate copolymer.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 5g of deionized water is added into a 100 mL three-neck flask, 1.00 g of dispersant BYK-111, 0.08 g of defoamer BYK-022 and 0.17 g of thickener UH-420 are added dropwise, and mechanical stirring is carried out for 40 min (the rotating speed is 800 r/min).
Preparing a component B: 30g of aqueous fluorocarbon resin is added into a beaker, 0.08 g of defoaming agent BYK-054 is added dropwise, and magnetons are added for electromagnetic stirring for 35 min.
10g of titanium dioxide is added into the component A, and the mixture is stirred evenly (the mechanical stirring is carried out for 120 min, and the rotating speed is 800 r/min).
Pouring the component B into the component A and continuously stirring; 1.2 g of film forming additive methyl glycol methyl ether acetate and 0.12 g of thickening agent BYK-410 are mixed and added into the mixed liquid of the component A and the component B, and the mixture is stirred for 50 min (the rotating speed is 500 r/min).
Preparing a component C: 0.10 g of wetting dispersant BYK-163 was added to 0.35 g of ionized water, and the mixture was stirred uniformly to prepare a dispersant solution. And (3) taking 0.06 g of modified graphene, carrying out ball milling in a planetary ball mill for 25 min, and carrying out ultrasonic dispersion for 35 min to obtain the modified graphene dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
3.0 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 30 min.
The obtained coating comprises the following components in percentage by weight: 58.64% of water-based fluorocarbon resin, 10.46% of water, 1.95% of dispersing agent, 0.20% of wetting dispersing agent, 0.31% of defoaming agent, 0.57% of thickening agent, 19.55% of titanium dioxide, 2.34% of film-forming assistant, 5.86% of curing agent and 0.12% of modified graphene.
Spray coating with a spray gun.
Comparative example 3
Comparative example 3 does not include a process for preparing modified graphene, and unmodified graphene is directly used. Otherwise, the material amount and the preparation process were the same as in example 3, to obtain a heavy duty anticorrosive paint.
Example 4
(1) Preparing modified graphene:
the monomers such as vinyl acetate, vinyl versatate and the like are purified by reduced pressure distillation. Tween-80 was dissolved in acetic acid/sodium acetate buffer at pH 3 to a concentration of 3X 10-3In mol/L Tween-80 solution. And (3) ball-milling 0.86 g of carbon nanotubes and 0.86 g of graphene in a planetary ball mill for 60 min, dissolving in 40 mL of the solution, and performing ultrasonic dispersion for 30 min. Then, 1.06 g of vinyl acetate and 0.38 g of vinyl acetate were added thereto, and the mixture was stirred at a high speed for 24 hours. Into the above solution0.60 g of ammonium persulfate is added, the temperature is raised, and the reaction lasts for 4 hours at 80 ℃. 160 mL of magnesium sulfate with the concentration of 35g/L is added for demulsification, filtration, washing and drying at 70 ℃ for 8 hours to obtain the modified graphene coated by the vinyl acetate-vinyl versatate copolymer.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 5g of deionized water is added into a 100 mL three-neck flask, 1.10 g of dispersant BYK-AT204, 0.06 g of defoaming agent BYK-065 and 0.12 g of thickener BYK-428 are added dropwise, and mechanical stirring is carried out for 40 min (rotating speed is 800 r/min).
Preparing a component B: 29g of aqueous fluorocarbon resin is added into a beaker, 0.14 g of defoaming agent BYK-A501 is added dropwise, and magnetons are added to carry out electromagnetic stirring for 40 min.
9g of titanium dioxide is added into the component A, and the mixture is stirred evenly (the mechanical stirring is carried out for 100 min, and the rotating speed is 700 r/min).
Pouring the component B into the component A and continuously stirring; mixing 1.0 g of film-forming aid alcohol ester twelve and 0.15 g of thickener BYK-410, adding into the mixed solution of the component A and the component B, and stirring for 40 min (rotating speed 600 r/min).
Preparing a component C: 0.14 g of wetting dispersant BYK-9077 is added into 0.50 g of deionized water, and the mixture is stirred uniformly to prepare dispersant solution. And (3) taking 0.15 g of modified graphene/carbon nano tube, carrying out ball milling in a planetary ball mill for 30 min, and carrying out ultrasonic dispersion for 35 min to obtain the modified graphene/carbon nano tube dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
2.5 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 40 min.
The obtained coating comprises the following components in percentage by weight: 59.35% of waterborne fluorocarbon resin, 11.26% of water, 2.25% of dispersant, 0.29% of wetting dispersant, 0.41% of defoaming agent, 0.55% of thickener, 18.42% of titanium dioxide, 2.04% of film-forming assistant, 5.12% of curing agent and 0.31% of modified graphene/carbon nano tube.
Spray coating with a spray gun.
Comparative example 4
Comparative example 4 did not include a process for preparing modified graphene, and unmodified graphene was directly used. Otherwise, the material amount and the preparation process were the same as in example 4, to obtain a heavy duty anticorrosive paint.
Example 5
(1) Preparing modified graphene/carbon nanotubes:
the monomers such as vinyl acetate, vinyl versatate and the like are purified by reduced pressure distillation. Sodium dodecylbenzenesulfonate was dissolved in acetic acid/sodium acetate buffer at pH 4 to prepare a 5X 10 concentration-3mol/L sodium dodecyl benzene sulfonate solution. And (3) taking 0.56 g of graphene and 1.16 g of carbon nanotubes, carrying out ball milling in a planetary ball mill for 20 min, dissolving in 50 mL of the solution, and carrying out ultrasonic dispersion for 40 min. Then, 2.76 g of vinyl acetate and 0.68 g of vinyl acetate were added and stirred at a high speed for 24 hours. 0.70 g of ammonium persulfate was added to the above solution, and the mixture was heated to 80 ℃ to react for 4 hours. Adding 180 mL of 30g/L magnesium sulfate for demulsification, filtering, washing, and drying at 70 ℃ for 8 h to obtain the modified graphene/carbon nano tube coated by the vinyl acetate-vinyl versatate copolymer.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 5g of deionized water is added into a 100 mL three-neck flask, 1.00 g of dispersant BYK-190, 0.08 g of defoamer BYK-A555 and 0.17 g of thickener BYK-420 are added dropwise, and mechanical stirring is carried out for 40 min (the rotating speed is 800 r/min).
Preparing a component B: 30g of aqueous fluorocarbon resin is added into a beaker, 0.08 g of defoaming agent BYK-A501 is added dropwise, and magnetons are added for electromagnetic stirring for 35 min.
9.5g of titanium dioxide is added into the component A and stirred evenly (mechanical stirring is carried out for 120 min, and the rotating speed is 800 r/min).
Pouring the component B into the mixed solution A and continuously stirring; 1.2 g of film-forming assistant butyl cellosolve and 0.12 g of thickening agent UH-420 are mixed and added into the mixed solution of the component A and the component B, and the mixture is stirred for 50 min (the rotating speed is 500 r/min).
Preparing a component C: 0.10 g of wetting dispersant BYK-168 was added to 0.35 g of deionized water and stirred uniformly to prepare a dispersant solution. And (3) taking 0.06 g of modified graphene/carbon nano tube, carrying out ball milling in a planetary ball mill for 25 min, and carrying out ultrasonic dispersion for 35 min to obtain the modified graphene/carbon nano tube dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
3.0 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 30 min.
The obtained coating comprises the following components in percentage by weight: 59.22% of waterborne fluorocarbon resin, 10.56% of water, 1.97% of dispersing agent, 0.20% of wetting dispersing agent, 0.32% of defoaming agent, 0.57% of thickening agent, 18.75% of titanium dioxide, 2.37% of film-forming assistant, 5.92% of curing agent and 0.12% of modified graphene-carbon nano tube.
Spray coating with a spray gun.
Comparative example 5
Comparative example 5 did not include a process for preparing modified graphene/carbon nanotubes, and unmodified graphene-carbon nanotubes were used directly. Otherwise, the material amount and the preparation process were the same as in example 5, to obtain a heavy duty anticorrosive paint.
Example 6
(1) Preparing modified graphene/carbon nanotubes:
and carrying out reduced pressure distillation purification on the vinyl acetate. KH-550 was dissolved in acetic acid/sodium acetate buffer at pH 3 to prepare a concentration of 4X 10-3mol/L KH-550 solution. Taking 1.16 g of graphene and 0.56 g of carbon nano tube, carrying out ball milling in a planetary ball mill for 15 min, dissolving in 40 mL of the solution, and carrying out ultrasonic dispersion for 50 min. 3.44 g of vinyl acetate was added thereto, and the mixture was stirred at high speed for 24 hours. 0.52 g of ammonium persulfate was added to the above solution, and the mixture was heated to 80 ℃ to react for 4 hours. Adding 200 mL of 35g/L magnesium sulfate for demulsification, filtering, washing, and drying at 70 ℃ for 8 h to obtain the polyvinyl acetate coated modified graphene/carbon nano tube.
(2) Preparing a heavy anti-corrosion coating:
preparing a component A: 4 g of deionized water is added into a 100 mL three-neck flask, 0.90 g of dispersant BYK-192, 0.06 g of defoaming agent BYK-021 and 0.15 g of thickening agent BYK-428 are dripped, and mechanical stirring is carried out for 25 min (the rotating speed is 700 r/min).
Preparing a component B: 22 g of waterborne fluorocarbon resin is added into a beaker, 0.10 g of defoaming agent BYK-141 is added dropwise, and magnetons are added for electromagnetic stirring for 40 min.
8g of titanium dioxide is added into the component A, and the mixture is stirred evenly (the mechanical stirring is carried out for 100 min, and the rotating speed is 900 r/min).
Pouring the component B into the mixed solution A and continuously stirring; 1.1 g of film forming additive methyl glycol methyl ether acetate and 0.15 g of thickening agent BYK-420 are mixed and added into the mixed liquid of the component A and the component B, and the mixture is stirred for 60 min (the rotating speed is 600 r/min).
Preparing a component C: 0.05 g of wetting dispersant BYK-P104 was added to 0.22 g of deionized water, and the mixture was stirred uniformly to prepare a dispersant solution. And (3) taking 0.05 g of modified graphene/carbon nano tube, carrying out ball milling in a planetary ball mill for 15 min, and carrying out ultrasonic dispersion for 30 min to obtain the modified graphene/carbon nano tube dispersion liquid.
Adding the component C into the component A and the component B, and electromagnetically stirring at a low speed until the components are uniform.
2.6 g of Nippon 4F curing agent is added into the mixed solution, and the mixture is stirred for 25 min.
The obtained coating comprises the following components in percentage by weight: 55.87% of waterborne fluorocarbon resin, 10.72% of water, 2.29% of dispersant, 0.12% of wetting dispersant, 0.41% of defoaming agent, 0.76% of thickener, 20.31% of titanium dioxide, 2.79% of film-forming assistant, 6.60% of curing agent and 0.13% of modified graphene-carbon nano tube.
Spray coating with a spray gun.
Comparative example 6
Comparative example 6 did not include a process for preparing modified graphene/carbon nanotubes, and unmodified graphene-carbon nanotubes were used directly. Otherwise, the material amount and the preparation process were the same as in example 6, to obtain a heavy duty anticorrosive paint.
And analyzing the performance indexes of the prepared modified graphene and the aqueous fluorocarbon resin heavy-duty anticorrosive paint of the modified graphene/carbon nano tube.
Measurement of Pencil hardness: the test is carried out according to the standard GB/T6379-2006 "determination of paint film hardness by color paint and varnish pencil method". Spraying a layer (25 +/-5 mu m) on a tin plate, curing for 7 days, pushing a pencil hardness tester on a paint film, and comparing the situation that when a pencil with specified hardness is pushed to pass through the surface of the paint film, the surface of the paint film is scratched. The hardness of the coating is expressed as the hardness of the hardest pencil in which the film is free of defects.
And (3) testing the adhesive force: testing according to standard GB/T5210-2006 adhesion test by paint and varnish pulling method. Spraying one (90 +/-10 mu m) layer on the tinplate, curing for 7 days, and adjusting for 16 h under the conditions of temperature (23 +/-2) DEG C and humidity (50 +/-5)%. After a small amount of adhesive is used for adhesion, a sample is placed on a proper tensile testing machine, tensile stress is applied in the direction vertical to the plane of the paint material, the stress is stably increased at a uniform speed not exceeding 1 Mpa/s, the damage process is completed within 90 s, and the tensile testing machine displays that the index is the adhesive force of the coating.
TABLE 1 main Properties of heavy duty anticorrosive coatings obtained in examples and comparative examples
Compared with unmodified graphene and graphene/carbon nanotube composite coatings, the modified graphene and modified graphene/carbon nanotube composite coatings are obviously improved in pencil hardness and adhesive force, and the polymer coated carbon material is proved to improve the compatibility between the carbon material and resin.
The foregoing embodiments are intended to illustrate that the invention may be implemented or used by those skilled in the art, and modifications to the above embodiments will be apparent to those skilled in the art, and therefore the invention includes, but is not limited to, the above embodiments, any methods, processes, products, etc., consistent with the principles and novel and inventive features disclosed herein, and fall within the scope of the invention.
Claims (13)
1. The water-based fluorocarbon resin heavy-duty anticorrosive paint comprises the following components in parts by mass:
50-60 wt% of water-based fluorocarbon resin, 8-15 wt% of water, 2-3% of dispersing agent, 0.1-1.0% of defoaming agent, 0.6-1.0% of thickening agent, 18-28% of titanium dioxide, 1-4% of film forming additive, 4-9% of curing agent, 0.1-3% of wetting dispersing agent, 0.1-3% of modified graphene or graphene-carbon nano tube, wherein the modified graphene or graphene-carbon nano tube is graphene or graphene/carbon nano tube coated by polymer.
2. The heavy anti-corrosion coating according to claim 1, wherein the content of the wetting dispersant is 0.1% -2%.
3. The heavy-duty anticorrosive paint according to claim 1, wherein the polymer is polyvinyl acetate or a vinyl acetate/vinyl versatate copolymer, and the content of the polymer in the modified graphene or graphene/carbon nanotubes is 1wt% to 20 wt%.
4. The heavy-duty anticorrosive paint as claimed in claim 1, wherein the dispersant is one or more selected from BYK-162, BYK-192, BYK-190, BYK-9076, BYK-111, BYK-AT204 and BYK-110; the defoaming agent is selected from one or more of BYK-A555, BYK-022, BYK-052, BYK-088, BYK-011, BYK-019 and BYK-065; the thickening agent is selected from one of BYK-420, BYK-425, UH-420, BYK-428, BYK-410 and BYK-A200; the film-forming assistant is selected from one or more of propylene glycol butyl ether, alcohol ester twelve and methyl glycol methyl ether acetate; the curing agent is selected from Nippon 4F curing agent.
5. The heavy-duty anticorrosive paint according to claim 1, wherein the modified graphene or modified graphene/carbon nanotube is prepared by the following method:
firstly, dissolving a surfactant in an acetic acid/sodium acetate buffer solution with the pH value of 3-5 to prepare a solution with the concentration of 3 multiplied by 10-3~6×10-3A surfactant solution in mol/L;
dispersing a proper amount of graphene or graphene/carbon nano tubes in a surfactant solution to obtain an emulsion;
adding monomer vinyl acetate or vinyl acetate/vinyl versatate into the emulsion obtained in the step two;
adding ammonium persulfate into the emulsion obtained in the step (III), wherein the mass of the ammonium persulfate is 15-35 wt% of the content of monomer vinyl acetate or vinyl acetate/vinyl versatate, heating and reacting;
demulsifying by using a magnesium sulfate solution, filtering, washing, and drying to obtain the polymer-coated modified graphene or graphene/carbon nanotubes.
6. The heavy-duty anticorrosive paint according to claim 5, wherein the step (r) further comprises an operation of purifying vinyl acetate and vinyl versatate monomers by distillation under reduced pressure.
7. The heavy-duty anticorrosive paint according to claim 5, wherein the graphene or graphene/carbon nanotubes are subjected to a grinding treatment before the step (II).
8. The heavy anti-corrosion coating as claimed in claim 5, wherein the step two is to perform ultrasonic dispersion for 30-80 min in the dispersion process.
9. The heavy-duty anticorrosive paint as claimed in claim 5, wherein the mass fraction of vinyl acetate in the vinyl acetate-vinyl versatate is 70wt% -90 wt%, and the mass fraction of the vinyl versatate is 10wt% -30 wt%.
10. The heavy-duty anticorrosive paint according to claim 5, wherein the mass ratio of graphene or graphene/carbon nanotubes to monomer vinyl acetate or vinyl acetate/vinyl versatate is (0-2): (8-10); the molar mass ratio of the total molar mass of the monomers to the surfactant is (0-3): (8-12).
11. The heavy-duty anticorrosive paint according to claim 5, wherein the mass concentration of the magnesium sulfate solution is 30-40 g/L.
12. The heavy-duty coating of claim 5, wherein said surfactant is selected from the group consisting of KH550 or OP-10, sodium dodecylbenzenesulfonate or Tween-80.
13. A method for preparing the heavy duty anticorrosive coating of any one of claims 1 to 12, comprising the steps of:
(1) adding water, a dispersing agent, a defoaming agent and a thickening agent according to a proportion, and uniformly mixing to obtain an A1 component; adding titanium dioxide, and continuously and uniformly mixing to obtain a component A;
(2) uniformly mixing the water-based fluorocarbon resin and the defoaming agent to obtain a component B; adding the component B into the component A, adding the film-forming assistant, and uniformly mixing;
(3) dispersing the modified graphene or graphene/carbon nano tube and an optional wetting dispersant to obtain a component C; adding the component C into the system obtained in the step (2), uniformly mixing, adding a curing agent, and uniformly mixing to obtain a heavy anti-corrosion coating;
wherein the modified graphene or graphene-carbon nanotube is polymer-coated graphene or graphene/carbon nanotube.
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