CN113861789A - Graphene modified epoxy-acrylic resin functional coating and preparation method thereof - Google Patents
Graphene modified epoxy-acrylic resin functional coating and preparation method thereof Download PDFInfo
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Images
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The graphene modified epoxy-acrylic resin functional coating is prepared from the following components in parts by mass: 0.04-0.16 part of modified graphene, 13-15 parts of water-based epoxy resin, 27-29 parts of water-based acrylic resin, 40-42 parts of functional filler, 1-1.2 parts of graphite, 18-20 parts of deionized water, 1.2-1.5 parts of film-forming additive, 1-1.2 parts of wetting agent, 0.7-0.9 part of defoaming agent, 0.8-1 part of curing agent, 0.4-0.6 part of thickening agent, 0.6-0.8 part of coupling agent and 0.2-0.3 part of pH regulator. The waterborne epoxy-acrylic resin coating prepared by the invention has the advantages of excellent corrosion resistance, wear resistance, adhesive force and hardness of the epoxy coating, excellent flexibility and weather resistance of the acrylic coating, high damping performance and lower cost.
Description
(I) technical field
The invention relates to a novel graphene modified epoxy-acrylic resin functional coating and a preparation method thereof.
(II) background of the invention
With the continuous progress of science and technology, the problems caused by vibration and noise are more and more of social concern. Vibration and noise not only limit the improvement of mechanical equipment performance, but also harm physical and mental health of people. The water-based damping coating is a preferred damping material for vibration and noise reduction because of convenient construction, environmental protection and low cost. However, with the wider application range and wider application places (such as being used for building outer walls, high-speed rail car bottoms and the like), higher requirements are put on the performances (such as weather resistance and mechanical properties) of the coating. The existing common damping coating has no functions of wear resistance, corrosion resistance, tensile resistance and the like, and can corrode or fall off when exposed to the external environment for a long time, so that the service life of equipment parts is further shortened due to the fact that the substrate is abraded.
The water-based epoxy-acrylic coating has the advantages of excellent corrosion resistance, wear resistance, adhesive force and hardness of the epoxy coating, and excellent flexibility and weather resistance of the acrylic coating, has wide application prospect in the field of coatings due to excellent comprehensive performance, but has relatively few application researches in the field of damping at present. On the other hand, due to the fact that the graphene is large in specific surface area and is of a sheet-like structure, gaps existing in resin can be filled after the resin is added, the graphene is stacked layer by layer, a path of a corrosive medium reaching the surface of a substrate can be prolonged, corrosion is delayed, and therefore the graphene can play a role in corrosion prevention. In addition, the graphene also has good mechanical properties such as toughness and the like, and can improve the mechanical properties of the coating. Therefore, the graphene and the water-based damping coating are combined, so that the effects of the graphene and the water-based damping coating can be fully exerted, the original damping performance can be guaranteed, and the coating can be endowed with good corrosion resistance, wear resistance and tensile resistance. However, the graphene added into the resin has the problems of poor dispersibility and poor compatibility, and further influences the corrosion resistance, wear resistance and damping performance of the coating.
Based on the method, the graphene is modified, the compatibility between the graphene and the waterborne epoxy resin and the waterborne acrylic resin is improved, the proportion of the epoxy resin and the acrylic resin is optimized, a novel multifunctional coating with corrosion resistance, wear resistance, tensile resistance and damping performance is developed, and the application field of the coating is further expanded.
(III) technical scheme
In order to solve the problems of poor dispersibility and poor compatibility of graphene added into resin in the prior art, the invention aims to provide a functional damping coating taking graphene modified epoxy-acrylic resin as a matrix and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a graphene modified epoxy-acrylic resin functional coating, which is prepared from the following components in parts by mass: 0.04-0.16 part (preferably 0.12 part) of modified graphene, 13-15 parts of waterborne epoxy resin, 27-29 parts of waterborne acrylic resin, 40-44 parts of functional filler, 1-1.2 parts of graphite, 18-20 parts of deionized water, 1.2-1.5 parts of film-forming additive, 1-1.2 parts of wetting agent, 0.7-0.9 part of defoaming agent, 0.8-1 part of curing agent, 0.4-0.6 part of thickening agent and 0.6-0.8 part of coupling agent;
the modified graphene is obtained by performing sand milling modification on an organic micromolecule modifier ethyl phenyl polyethylene glycol (NP-40); based on the total mass of all components of the graphene modified epoxy-acrylic resin functional coating, the functional filler is composed of 27-28 parts of mica, 8-10 parts of talcum powder and 5-6 parts of calcium carbonate; the wetting agent is a nonionic surfactant; the defoaming agent is an acrylic defoaming agent; the curing agent is a water-based epoxy curing agent; the coupling agent is a silane coupling agent; the thickening agent is a span cellulose thickening agent.
Further, the film-forming aid is Islam twelve.
Specifically, the modified graphene is prepared according to the following method: weighing organic micromolecule modifier ethyl phenyl polyethylene glycol and absolute ethyl alcohol, and stirring and dissolving to obtain a modification solution; adding graphene powder and deionized water; starting a high-speed stirrer, stirring at 600-700r/min for 5-6min (preferably stirring at 600r/min for 5min), then opening a sand mill, and sanding at 1100-1200r/min for 15-20min (preferably sanding at 1200r/min for 18 min); drying the obtained slurry to obtain the modified graphene; the mass ratio of the organic micromolecule modifier ethyl phenyl polyethylene glycol, absolute ethyl alcohol, graphene powder and deionized water is 0.9-1: 90-95: 30-32: 1800-1900.
Specifically, the coupling agent is a silane coupling agent KH-550 or KH-560 (preferably KH-560); the thickener is a sublibrillar cellulose thickener HBR 250.
Furthermore, the water-based acrylic resin is milky blue liquid with the solid content of 55%, the viscosity of 100-500cps and the glass transition temperature of-10 ℃, and is preferably pure acrylic emulsion.
Further, the solid content of the waterborne epoxy resin is 55 percent, the viscosity is 500-2000cps, the epoxy equivalent is 300-360eq/g, the appearance is white uniform liquid, and the waterborne epoxy resin is preferably waterborne epoxy emulsion GS-740A.
Further, the curing agent has the solid content of 50 percent, the viscosity of 5000-7000cps and the appearance of yellow translucent uniform liquid, and is preferably waterborne epoxy curing agent GS-740B.
Further, the graphene modified epoxy-acrylic resin is prepared by modifying graphene, blending the modified graphene with epoxy resin, and then blending the modified graphene with acrylic resin.
Further, the wetting agent is preferably a wetting agent of Runtai PE-100 or DX200 (preferably wetting agent of Runtai DX 200).
Further, the defoaming agent is preferably a high-efficiency broad-spectrum liquid defoaming agent NXZ.
Preferably, the graphene modified epoxy-acrylic resin functional coating is prepared from the following components in parts by mass: 0.12 part of modified graphene, 14 parts of waterborne epoxy resin, 28 parts of waterborne acrylic resin, 42 parts of functional filler, 1.1 parts of graphite, 18 parts of deionized water, 1.4 parts of film-forming additive, 1.2 parts of wetting agent, 0.8 part of defoaming agent, 0.8 part of curing agent, 0.4 part of thickening agent and 0.7 part of coupling agent.
Further preferably, the graphene modified resin-based functional coating is prepared from the following components in parts by mass: 0.12 part of modified graphene powder, 14 parts of waterborne epoxy resin, 28 parts of waterborne acrylic resin, 42 parts of functional filler (preferably 27 parts of mica, 10 parts of talcum powder and 5 parts of calcium carbonate), 1.1 parts of graphite, 18 parts of deionized water, 1.4 parts of film-forming additive Islam alcohol ester, DX 2001.2 parts of Runtai wetting agent, 0.8 part of defoaming agent NXZ, 0.8 part of curing agent, 2500.4 parts of Sulfolone hydroxyethyl cellulose thickener and KH-5600.7 parts of silane coupling agent.
Further, the graphene modified epoxy-acrylic resin functional coating is prepared by the following method: weighing the water-based epoxy emulsion with the formula amount in a beaker, adding the modified graphene with the formula amount, mechanically fully stirring for reaction, adding the water-based acrylate emulsion with the formula amount, uniformly mixing, sequentially and uniformly mixing the wetting agent and the defoaming agent with the formula amount, adjusting the pH value to be neutral by using a pH regulator (usually AMP-95), adding the film-forming assistant with the formula amount, and fully stirring to obtain water-based emulsion a; uniformly stirring the deionized water and the functional filler in the component amount, adding the graphite in the component amount, continuously stirring, adding the silane coupling agent in the component amount, and fully stirring to obtain an aqueous solution b; and adding the aqueous solution b into the aqueous emulsion a, uniformly mixing under high-speed stirring, adding a formula amount of aqueous epoxy curing agent and a thickening agent, and fully stirring to obtain the graphene modified epoxy-acrylic resin functional coating.
In a second aspect, the invention further provides a preparation method of the graphene modified epoxy-acrylic resin functional coating, wherein the method comprises the following steps:
(1) preparing modified graphene: weighing organic micromolecule modifier ethyl phenyl polyethylene glycol and absolute ethyl alcohol, and stirring and dissolving to obtain a modification solution; adding graphene powder and deionized water; starting a high-speed stirrer, stirring at 600-700r/min for 5-6min (preferably stirring at 600r/min for 5min), then opening a sand mill, and sanding at 1100-1200r/min for 15-20min (preferably sanding at 1200r/min for 18 min); drying the obtained slurry to obtain the modified graphene; the mass ratio of the organic micromolecule modifier ethyl phenyl polyethylene glycol, absolute ethyl alcohol, graphene powder and deionized water is 0.9-1: 90-95: 30-32: 1800-1900;
(2) weighing the water-based epoxy emulsion with the formula amount in a beaker, adding the modified graphene prepared in the step (1) with the formula amount, mechanically stirring and reacting for 1-2h at 400r/min of 300-;
(3) taking another amount of deionized water, adding the functional filler in the amount of the group, stirring for 15-20min (preferably stirring for 20min at 600 r/min) at 500-;
(4) adding the aqueous solution b obtained in the step (3) into the aqueous emulsion a obtained in the step (2), stirring at a high speed of 1500-;
based on the total mass of all components of the graphene modified epoxy-acrylic resin functional coating, the functional filler is composed of 27-28 parts of mica, 8-10 parts of talcum powder and 5-6 parts of calcium carbonate; the wetting agent is a nonionic surfactant; the defoaming agent is an acrylic defoaming agent; the curing agent is a water-based epoxy curing agent; the coupling agent is a silane coupling agent; the thickening agent is a span cellulose thickening agent.
Further, the film-forming aid is Islam twelve.
Specifically, the coupling agent is a silane coupling agent KH-550 or KH-560 (preferably KH-560); the thickener is a sublibrillar cellulose thickener HBR 250.
Furthermore, the water-based acrylic resin is milky blue liquid with the solid content of 55%, the viscosity of 100-500cps and the glass transition temperature of-10 ℃, and is preferably pure acrylic emulsion.
Further, the solid content of the waterborne epoxy resin is 55 percent, the viscosity is 500-2000cps, the epoxy equivalent is 300-360eq/g, the appearance is white uniform liquid, and the waterborne epoxy resin is preferably waterborne epoxy emulsion GS-740A.
Further, the curing agent has the solid content of 50 percent, the viscosity of 5000-7000cps and the appearance of yellow translucent uniform liquid, and is preferably waterborne epoxy curing agent GS-740B.
Further, the graphene modified epoxy-acrylic resin is prepared by modifying graphene, blending the modified graphene with epoxy resin, and then blending the modified graphene with acrylic resin.
Further, the wetting agent is preferably a wetting agent of Runtai PE-100 or DX200 (preferably wetting agent of Runtai DX 200).
Further, the defoaming agent is preferably a high-efficiency broad-spectrum liquid defoaming agent NXZ.
Preferably, the graphene modified epoxy-acrylic resin functional coating is prepared from the following components in parts by mass: 0.12 part of modified graphene, 14 parts of waterborne epoxy resin, 28 parts of waterborne acrylic resin, 42 parts of functional filler, 1.1 parts of graphite, 18 parts of deionized water, 1.4 parts of film-forming additive, 1.2 parts of wetting agent, 0.8 part of defoaming agent, 0.8 part of curing agent, 0.4 part of thickening agent and 0.7 part of coupling agent.
Further preferably, the graphene modified resin-based functional coating is prepared from the following components in parts by mass: 0.12 part of modified graphene powder, 14 parts of waterborne epoxy resin, 28 parts of waterborne acrylic resin, 42 parts of functional filler (preferably 27 parts of mica, 10 parts of talcum powder and 5 parts of calcium carbonate), 1.1 parts of graphite, 18 parts of deionized water, 1.4 parts of film-forming additive Islam alcohol ester, DX 2001.2 parts of Runtai wetting agent, 0.8 part of defoaming agent NXZ, 0.8 part of curing agent, 2500.4 parts of Sulfolone hydroxyethyl cellulose thickener and KH-5600.7 parts of silane coupling agent.
Compared with the prior art, the invention has the following beneficial effects:
(1) the waterborne epoxy-acrylic resin obtained by blending and modifying the epoxy resin and the acrylic resin can have the excellent corrosion resistance, wear resistance, adhesive force and hardness of the epoxy resin and the excellent flexibility and weather resistance of the acrylic resin.
(2) By adding an organic micromolecule sanding modification method, pi-pi conjugation effect is generated between the micromolecule electron cloud and the graphene electron cloud, and the aggregate of the graphene is broken. And the modified graphene can also have the effect with resin through hydrogen bond effect and the like, so that the surface bonding is reduced and the agglomeration is reduced, and the dispersibility of the graphene in the resin matrix is improved. The diaphragm formed by using the lamellar graphene has good physical barrier property, has the advantages of good corrosion resistance, friction resistance and high strength, further improves the corrosion resistance, friction resistance and tensile resistance of the coating, and finally obtains the novel functional coating with damping, corrosion resistance, wear resistance and tensile resistance.
Drawings
FIG. 1 is a diagram of damping performance of functional coating with different contents of graphene/epoxy-acrylic resin
FIG. 2 is a Nyquist impedance diagram of functional coatings with different contents of graphene/epoxy-acrylic resin
FIG. 3 is a Tafel polarization curve of functional coating with different contents of graphene/epoxy-acrylic resin
FIG. 4 is a graph of the wear resistance of functional coatings with different contents of graphene/epoxy-acrylic resin
FIG. 5 is a stress-strain curve of graphene/epoxy-acrylic resin functional coating with different contents
Detailed Description
The invention will now be further illustrated by the following examples, without limiting the scope of the invention thereto.
The damping performance was measured using a British dynamic thermomechanical analyzer (DMA8000), samples were cut at 10mm 2mm, the temperature range was-40 ℃ to 80 ℃, the rate of temperature rise was 3 ℃/min, and the frequency was 2 Hz.
The impedance and Tafel polarization curves are tested by using an electrochemical workstation, and a three-electrode system is adopted, wherein the sample is a working electrode, and the area of the sample is 1cm2The test solution is uniformly coated on a carbon steel sheet, a 3M glue edge is used for sealing, saturated calomel is selected as a reference electrode, a platinum wire is selected as an auxiliary electrode, and an electrochemical test medium is 3.5% NaCl solution. The frequency range of impedance test is 10-2-105Hz, the disturbance signal is a 20mV sine wave. The Tafel polarization curve is tested to be in a voltage range of-1.0-0.2V, and the scanning speed is 0.2 mV/s.
According to GB/T1768-2006, the wear resistance of the coating is measured by rubbing the paint film by a rubber grinding wheel fixed on a wear tester, and the mass loss of the paint film after a specified number of rubbing cycles is expressed, wherein the weight on the rubber grinding wheel is 750g, and the rotating speed is 60 r/min.
The mechanical property adopts a universal tensile machine, the GB/T528-2009 standard is adopted for testing, the test sample is an I-type dumbbell-shaped test sample D grade, the test length is 25.0 +/-0.5 mm, and the tensile rate is 500 +/-50 mm/min.
Small molecule ethyl phenyl polyethylene glycol, Ron's reagent; water-based epoxy emulsion GS-740A, water-based epoxy curing agent GS-740B, Guangzhou Guangshu chemical technology Co., Ltd; water acrylic ester emulsion (pure acrylic), graphene, Qingdao Haiyuan industry Co.
Example 1
Firstly, 0.9g of micromolecule ethyl phenyl polyethylene glycol is weighed in a beaker, 90g of absolute ethyl alcohol is added, and the modification solution is obtained after stirring and dissolving. 30g of graphene powder is weighed in a plastic bucket, the prepared modification liquid is added, and 1800g of deionized water is added. Starting the high-speed stirrer, wherein the rotating speed is 600r/min, the stirring time is 5min, and then starting the sand mill, wherein the rotating speed is 1200r/min, and the sand milling time is 18 min. And drying the obtained slurry to obtain the modified graphene.
Weighing 14g of water-based epoxy emulsion in a beaker, adding 0.04g of prepared modified graphene, mechanically stirring for reaction for 1h at 400r/min, then adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at 800r/min, then sequentially adding 1.2g of Runtai wetting agent DX200 and 0.8g of defoaming agent NXZ, adding pH regulator AMP-95 until the pH is neutral, then adding 1.4g of film-forming aid Islam alcohol ester dodeca, and stirring for 10min at 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, putting the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of aqueous epoxy curing agent and 0.4g of Subspan hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the graphene modified epoxy-acrylic resin functional coating.
Example 2
Firstly, 0.9g of micromolecule ethyl phenyl polyethylene glycol is weighed in a beaker, 90g of absolute ethyl alcohol is added, and the modification solution is obtained after stirring and dissolving. 30g of graphene powder is weighed in a plastic bucket, the prepared modification liquid is added, and 1800g of deionized water is added. Starting the high-speed stirrer, wherein the rotating speed is 600r/min, the stirring time is 5min, and then starting the sand mill, wherein the rotating speed is 1200r/min, and the sand milling time is 18 min. And drying the obtained slurry to obtain the modified graphene.
Weighing 14g of water-based epoxy emulsion in a beaker, adding 0.08g of prepared modified graphene, mechanically stirring for reaction for 1h at 400r/min, then adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at 800r/min, then sequentially adding 1.2g of Runtai wetting agent DX200 and 0.8g of defoaming agent NXZ, adding pH regulator AMP-95 until the pH is neutral, then adding 1.4g of film-forming aid Islam alcohol ester dodeca, and stirring for 10min at 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, putting the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of aqueous epoxy curing agent and 0.4g of Subspan hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the graphene modified epoxy-acrylic resin functional coating.
Example 3
Firstly, 0.9g of micromolecule ethyl phenyl polyethylene glycol is weighed in a beaker, 90g of absolute ethyl alcohol is added, and the modification solution is obtained after stirring and dissolving. 30g of graphene powder is weighed in a plastic bucket, the prepared modification liquid is added, and 1800g of deionized water is added. Starting the high-speed stirrer, wherein the rotating speed is 600r/min, the stirring time is 5min, and then starting the sand mill, wherein the rotating speed is 1200r/min, and the sand milling time is 18 min. And drying the obtained slurry to obtain the modified graphene.
Weighing 14g of water-based epoxy emulsion in a beaker, adding 0.12g of prepared modified graphene, mechanically stirring for reaction for 1h at 400r/min, then adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at 800r/min, then sequentially adding 1.2g of Runtai wetting agent DX200 and 0.8g of defoaming agent NXZ, adding pH regulator AMP-95 until the pH is neutral, then adding 1.4g of film-forming aid Islam alcohol ester dodeca, and stirring for 10min at 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, placing the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of curing agent and 0.4g of Suanlong hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the graphene modified epoxy-acrylic resin functional coating.
Example 4
Firstly, 0.9g of micromolecule ethyl phenyl polyethylene glycol is weighed in a beaker, 90g of absolute ethyl alcohol is added, and the modification solution is obtained after stirring and dissolving. 30g of graphene powder is weighed in a plastic bucket, the prepared modification liquid is added, and 1800g of deionized water is added. Starting the high-speed stirrer, wherein the rotating speed is 600r/min, the stirring time is 5min, and then starting the sand mill, wherein the rotating speed is 1200r/min, and the sand milling time is 18 min. And drying the obtained slurry to obtain the modified graphene.
Weighing 14g of water-based epoxy emulsion in a beaker, adding 0.16g of prepared modified graphene, mechanically stirring for reaction for 1h at 400r/min, then adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at 800r/min, then sequentially adding 1.2g of Runtai wetting agent DX200 and 0.8g of defoaming agent NXZ, adding pH regulator AMP-95 until the pH is neutral, then adding 1.4g of film-forming aid Islam alcohol ester dodeca, and stirring for 10min at 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, putting the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of aqueous epoxy curing agent and 0.4g of Subspan hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the graphene modified epoxy-acrylic resin functional coating.
Comparative example 1
The preparation method of the common water-based damping paint is as follows:
weighing 14g of water-based epoxy emulsion in a beaker, adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at the speed of 800r/min, sequentially adding 1.2g of a Runtai wetting agent DX200 and 0.8g of a defoaming agent NXZ, adding a pH regulator AMP-95 to be neutral, adding 1.4g of a film-forming aid Islam twelve, and stirring for 10min at the speed of 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, putting the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of aqueous epoxy curing agent and 0.4g of Subspan hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the epoxy-acrylic resin functional coating.
Comparative example 2
Weighing 14g of water-based epoxy emulsion in a beaker, adding 0.04g of unmodified graphene, mechanically stirring for reaction for 1h at the speed of 400r/min, then adding 28g of water-based acrylate emulsion, mechanically stirring for 30min at the speed of 800r/min, then sequentially adding 1.2g of Runtai wetting agent DX200 and 0.8g of defoaming agent NXZ, adding pH regulator AMP-95 to be neutral, then adding 1.4g of film-forming aid Islam twelve, and stirring for 10min at the speed of 600r/min to obtain water-based emulsion a;
then taking 18g of deionized water, adding 42g of functional filler (27 g of mica, 10g of talcum powder and 5g of calcium carbonate) and stirring for 20min at 600r/min, then adding 1.1g of graphite and continuing to stir for 5min at 600r/min, then adding 0.7g of silane coupling agent KH-560 and stirring for 35min at 700r/min to obtain aqueous solution b;
and adding the aqueous solution b into the aqueous emulsion a, putting the aqueous solution b into a mechanical stirring kettle, stirring at a high speed of 1600r/min for 30min, then adding 0.8g of aqueous epoxy curing agent and 0.4g of Subspan hydroxyethyl cellulose thickener HBR250, and stirring for about 10min to obtain the graphene modified epoxy-acrylic resin functional coating.
Through the graph 1, it can be found that after the modified graphene is added, the glass transition temperature corresponding to the damping coating is increased, and when the addition amount is 0.12 part, the loss factor is increased from 1.03 to 1.10, and the maximum value is reached; when the amount is increased to 0.16 part, the amount is reduced due to agglomeration, but the damping performance of the graphene modified acrylic resin functional coating is improved.
The influence on the coating impedance after the modified graphene is added can be found through the graph in fig. 2, the impedance values corresponding to the coating after the modified graphene is added are all improved, and when the addition amount of the modified graphene in example 3 is 0.12 parts, the impedance radius reaches the maximum, and the anticorrosion effect is improved obviously. However, when the amount of the modified graphene is 0.16 parts, agglomeration occurs due to van der waals force interaction between graphene sheets, and new voids are formed in the coating film, resulting in a decrease in anti-corrosive performance.
It is found from FIG. 3(Tafel polarization curve) that the self-corrosion current I increases with the amount of modified graphenecorrReduced, self-etching potential EcorrThe larger the size, the better the antiseptic effect. When the amount is increased to 0.12 part, the self-etching current IcorrIs 1.513 x 10-7A/cm2Self-etching potential EcorrIs-0.5178V, the most obvious anticorrosion performance. The anticorrosion performance of the graphene/epoxy-acrylic resin functional coating is well improved.
As can be seen from fig. 4, as the content of graphene in the resin increases, the amount of frictional wear thereof decreases correspondingly, and the wear resistance is effectively improved. The abrasion condition of the original damping coating is 48.5mg, the abrasion condition of the coating is reduced along with the increment of the graphene amount, the optimal 42.1mg is reached when the equivalent is 0.12 part, and then the coating is stabilized.
From fig. 5, it can be seen that the tensile strength and the elongation at break of the coating are improved after different contents of graphene are added, and the tensile strength reaches 3.79MPa at most when the content of graphene is 0.12 parts, and the elongation at break is 140.4%. Through analysis, the interaction between the oxygen-containing functional groups on the surface of the graphene and the polar bonds of the polymer mainly plays a certain role in enhancing the stability of the polymer chain, so that the mechanical property of the whole composite material is improved.
From all the figures we can also see that the addition of modified graphene is better than the unmodified performance.
In the above embodiments, any modification, equivalence, replacement improvement, etc. of the filler ratio and processing method according to the present invention to verify the two characteristics of corrosion resistance and damping of the paint are included in the protection scope of the present invention.
Claims (10)
1. A graphene modified epoxy-acrylic resin functional coating is characterized in that: the graphene modified epoxy-acrylic resin functional coating is prepared from the following components in parts by mass: 0.04-0.16 part of modified graphene, 13-15 parts of waterborne epoxy resin, 27-29 parts of waterborne acrylic resin, 40-44 parts of functional filler, 1-1.2 parts of graphite, 18-20 parts of deionized water, 1.2-1.5 parts of film-forming additive, 1-1.2 parts of wetting agent, 0.7-0.9 part of defoaming agent, 0.8-1 part of curing agent, 0.4-0.6 part of thickening agent and 0.6-0.8 part of coupling agent;
the modified graphene is obtained by performing sand grinding modification on an organic micromolecule modifier ethyl phenyl polyethylene glycol; based on the total mass of all components of the graphene modified epoxy-acrylic resin functional coating, the functional filler is composed of 27-28 parts of mica, 8-10 parts of talcum powder and 5-6 parts of calcium carbonate; the wetting agent is a nonionic surfactant; the defoaming agent is an acrylic defoaming agent; the curing agent is a water-based epoxy curing agent; the coupling agent is a silane coupling agent; the thickening agent is a span cellulose thickening agent.
2. The graphene-modified epoxy-acrylic resin functional coating of claim 1, wherein: the film-forming aid is Ismanol ester twelve.
3. The graphene-modified epoxy-acrylic resin functional coating according to claim 1 or 2, wherein the modified graphene is prepared according to the following method: weighing organic micromolecule modifier ethyl phenyl polyethylene glycol and absolute ethyl alcohol, and stirring and dissolving to obtain a modification solution; adding graphene powder and deionized water; starting the high-speed stirrer, stirring for 5-6min at the speed of 600-; drying the obtained slurry to obtain the modified graphene; the mass ratio of the organic micromolecule modifier ethyl phenyl polyethylene glycol, absolute ethyl alcohol, graphene powder and deionized water is 0.9-1: 90-95: 30-32: 1800-1900.
4. The graphene-modified epoxy-acrylic resin functional coating of claim 1, wherein: the water-based acrylic resin is pure acrylic emulsion.
5. The graphene-modified epoxy-acrylic resin functional coating of claim 1, wherein: the waterborne epoxy resin is waterborne epoxy emulsion GS-740A.
6. The graphene-modified epoxy-acrylic resin functional coating of claim 1, wherein: the curing agent is a waterborne epoxy curing agent GS-740B; the wetting agent is a Runtai wetting agent PE-100 or DX 200; the defoaming agent is a defoaming agent NXZ.
7. The graphene-modified epoxy-acrylic resin functional coating of claim 1, wherein: the coupling agent is a silane coupling agent KH-550 or KH-560; the thickener is a sublibrillar cellulose thickener HBR 250.
8. The graphene-modified epoxy-acrylic resin functional coating according to claim 1, wherein the graphene-modified epoxy-acrylic resin functional coating is prepared by the following method: weighing the water-based epoxy emulsion with the formula amount in a beaker, adding the modified graphene with the formula amount, mechanically fully stirring for reaction, adding the water-based acrylate emulsion with the formula amount, uniformly mixing, sequentially and uniformly mixing the wetting agent and the defoaming agent with the formula amount, adjusting the pH value to be neutral by using the pH regulator, adding the film-forming assistant with the formula amount, and fully stirring to obtain water-based emulsion a; uniformly stirring the deionized water and the functional filler in the component amount, adding the graphite in the component amount, continuously stirring, adding the silane coupling agent in the component amount, and fully stirring to obtain an aqueous solution b; and adding the aqueous solution b into the aqueous emulsion a, uniformly mixing under high-speed stirring, adding a formula amount of aqueous epoxy curing agent and a thickening agent, and fully stirring to obtain the graphene modified epoxy-acrylic resin functional coating.
9. The preparation method of the graphene-modified epoxy-acrylic resin functional coating according to claim 1, wherein the method comprises the following steps:
(1) preparing modified graphene: weighing organic micromolecule modifier ethyl phenyl polyethylene glycol and absolute ethyl alcohol, and stirring and dissolving to obtain a modification solution; adding graphene powder and deionized water; starting the high-speed stirrer, stirring for 5-6min at the speed of 600-; drying the obtained slurry to obtain the modified graphene; the mass ratio of the organic micromolecule modifier ethyl phenyl polyethylene glycol, absolute ethyl alcohol, graphene powder and deionized water is 0.9-1: 90-95: 30-32: 1800-1900;
(2) weighing the water-based epoxy emulsion with the formula amount in a beaker, adding the modified graphene prepared in the step (1) with the formula amount, mechanically stirring for reaction for 1-2h at 400r/min of 300-;
(3) taking deionized water with a formula amount, firstly adding functional filler with a formula amount, stirring for 15-20min at 600r/min under 500-;
(4) adding the aqueous solution b obtained in the step (3) into the aqueous emulsion a obtained in the step (2), stirring at a high speed of 1500-;
based on the total mass of all components of the graphene modified epoxy-acrylic resin functional coating, the functional filler is composed of 27-28 parts of mica, 8-10 parts of talcum powder and 5-6 parts of calcium carbonate; the wetting agent is a nonionic surfactant; the defoaming agent is an acrylic defoaming agent; the curing agent is a water-based epoxy curing agent; the coupling agent is a silane coupling agent; the thickening agent is a span cellulose thickening agent.
10. The method for preparing the graphene-modified epoxy-acrylic resin functional coating according to claim 9, wherein: the film-forming additive is Ismannite dodeca, the coupling agent is a silane coupling agent KH-550 or KH-560, and the water-based acrylic resin is a pure acrylic emulsion; the waterborne epoxy resin is waterborne epoxy emulsion GS-740A; the curing agent is a waterborne epoxy curing agent GS-740B; the wetting agent is a Runtai wetting agent PE-100 or DX 200; the defoaming agent is a defoaming agent NXZ; the pH regulator is AMP-95.
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