CN111484788A - Heat-dissipation coating of water-based carbon nanotube/epoxy resin dispersion system and preparation method and application thereof - Google Patents
Heat-dissipation coating of water-based carbon nanotube/epoxy resin dispersion system and preparation method and application thereof Download PDFInfo
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- CN111484788A CN111484788A CN202010319408.0A CN202010319408A CN111484788A CN 111484788 A CN111484788 A CN 111484788A CN 202010319408 A CN202010319408 A CN 202010319408A CN 111484788 A CN111484788 A CN 111484788A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/04—Epoxynovolacs
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides a heat dissipation coating of a water-based carbon nano tube/epoxy resin dispersion system, a preparation method and application thereof, and relates to the technical field of water-based coatings. The invention provides a water-based carbon nanotube/epoxy resin dispersion system heat dissipation coating which comprises the following components in parts by mass: 10-20 parts of water-based epoxy resin, 5-15 parts of hydrophilic carbon nano tubes, 5-20 parts of hydrophilic kaolin, 0-10 parts of water, 1-5 parts of defoaming agent, 1-5 parts of flatting agent and 3-10 parts of two-component water-based epoxy resin curing agent. The hydrophilic carbon nanotubes in the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system have good dispersibility and excellent heat dissipation performance, and can solve the technical problem of poor heat dissipation performance of the conventional heat conduction coating caused by poor dispersibility of the carbon nanotubes.
Description
Technical Field
The invention relates to the technical field of water-based paint, in particular to a heat dissipation paint of a water-based carbon nano tube/epoxy resin dispersion system, and a preparation method and application thereof.
Background
With the development of modern technology, various electronic components gradually tend to be miniaturized and highly efficient, and because electronic components generally have the characteristics of small size, long continuous working time and closed working environment, along with the continuous improvement of the input power of the electronic components, the heat flow density of the electronic components is very high, and the heat generation is large. If the heat cannot be dissipated in time, the temperature of the electronic product or local parts of the electronic product is too high, so that the service life of the capacitor is greatly shortened, the working performance is reduced, and the resource waste is caused. Therefore, the heat-conducting coating is coated on the surface of the electronic element, which solves the heat dissipation problem of the electronic element and ensures the normal work of the electronic element, and becomes a key means for restricting the development and application of the electronic technology.
In recent years, composite materials of carbon nanotubes and epoxy resin are widely used for solving the heat dissipation problem, the carbon nanotubes have good heat transfer performance, but the specific surface area and the length-diameter ratio of the carbon nanotubes are large, the surface of the carbon nanotubes is smooth and highly polarizable, large van der waals force action exists among aggregated tube bundles, the carbon nanotubes are extremely easy to agglomerate or tangle, the carbon nanotubes are difficult to uniformly disperse in the epoxy resin, and the heat dissipation performance of the heat-conducting coating is severely limited.
Disclosure of Invention
In view of the above, the invention provides a heat-dissipating coating material of an aqueous carbon nanotube/epoxy resin dispersion system, and a preparation method and application thereof. The heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system provided by the invention has excellent heat dissipation performance, and can solve the problem of poor heat dissipation performance of the conventional heat conduction coating.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a heat dissipation coating of a water-based carbon nano tube/epoxy resin dispersion system, which comprises the following components in parts by mass:
10-20 parts of water-based epoxy resin, 5-15 parts of hydrophilic carbon nano tubes, 5-20 parts of hydrophilic kaolin, 0-10 parts of water, 1-5 parts of defoaming agent, 1-5 parts of flatting agent and 3-10 parts of two-component water-based epoxy resin curing agent.
Preferably, the hydrophilic carbon nanotube is prepared by mixing raw materials including a carbon nanotube, an anionic surfactant, a phase transfer catalyst, a dispersant and water and performing a modification reaction;
the mass ratio of the carbon nano tube, the anionic surfactant, the phase transfer catalyst and the dispersing agent is (1-2): (1-2): (0.5-1): (3-5).
Preferably, the particle size of the hydrophilic carbon nano tube is 0.01-1 μm.
Preferably, the hydrophilic kaolin is prepared by mixing calcined kaolin, an anionic surfactant, a phase transfer catalyst, a dispersant and water and performing modification reaction;
the mass ratio of the calcined kaolin to the anionic surfactant to the phase transfer catalyst to the dispersant is (1-2): (1-2): (0.5-1): (3-5).
Preferably, the particle size of the hydrophilic kaolin is 0.01-1 μm.
Preferably, the aqueous epoxy resin preferably includes one or more of bisphenol a type epoxy resin, novolac type epoxy resin, and glycidyl ether type epoxy resin.
Preferably, the defoamer comprises one or more of tributyl phosphate, polyether defoamer and silicone defoamer.
Preferably, the leveling agent includes one or more of a polyurethane leveling agent, an organosilicon leveling agent, and an acrylic leveling agent.
The invention also provides a preparation method of the heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system, which comprises the following steps:
and sequentially mixing the water-based epoxy resin, the hydrophilic carbon nano tube, the hydrophilic kaolin, water, the defoaming agent, the leveling agent and the double-component water-based epoxy curing agent to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
The invention also provides the application of the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system in the technical scheme or the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system prepared by the preparation method in the technical scheme in a metal heat-dissipating product.
The invention provides a heat dissipation coating of a water-based carbon nano tube/epoxy resin dispersion system, which comprises the following components in parts by mass: 10-20 parts of water-based epoxy resin, 5-15 parts of hydrophilic carbon nano tubes, 5-20 parts of hydrophilic kaolin, 0-10 parts of water, 1-5 parts of defoaming agent, 1-5 parts of flatting agent and 3-10 parts of two-component water-based epoxy resin curing agent. The hydrophilic carbon nano tube is filled into the aqueous epoxy resin and can be uniformly dispersed in the aqueous epoxy resin, so that the heat conducting property and the heat conducting property of the heat dissipation coating of the aqueous carbon nano tube/epoxy resin dispersion system are effectively improved, the heat exchange efficiency is accelerated, and the heat conducting and heat dissipation efficiency is improved. In the invention, the hydrophilic kaolin has excellent bonding property, mechanical property and heat conduction property, the surface of the hydrophilic kaolin also has hydroxyl, sulfonic group and a small amount of amino hydrophilic groups, the hydrophilic kaolin has good hydrophilicity and high dispersibility in the heat dissipation coating. Meanwhile, due to the tubular structure of the hydrophilic carbon nano tube and the layered structure of the hydrophilic kaolin, the contact area of the two components in the aqueous epoxy resin is increased, a synergistic effect is generated, a perfect heat conducting network is formed, the heat conducting performance of the heat radiating coating of the aqueous carbon nano tube/epoxy resin dispersion system is effectively improved, and the reduction of the mechanical performance can be reduced. Therefore, the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system provided by the invention has excellent heat dissipation performance, and can solve the problem of poor heat dissipation performance of the conventional heat conduction coating. The raw materials of the heat dissipation coating of the water-based carbon nano tube/epoxy resin dispersion system provided by the invention are environment-friendly, and the discharge amount of VOC (volatile organic compounds) of the heat dissipation coating of the prepared water-based carbon nano tube/epoxy resin dispersion system is small.
Drawings
FIG. 1 is a diagram showing the thermal conductivity of the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion prepared in example 1;
fig. 2 is a relative radiation energy spectrum of the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system prepared in example 1.
Detailed Description
The invention provides a heat dissipation coating of a water-based carbon nano tube/epoxy resin dispersion system, which comprises the following components in parts by mass:
10-20 parts of water-based epoxy resin, 5-15 parts of hydrophilic carbon nano tubes, 5-20 parts of hydrophilic kaolin, 0-10 parts of water, 1-5 parts of defoaming agent, 1-5 parts of flatting agent and 3-10 parts of two-component water-based epoxy resin curing agent.
In the present invention, the raw materials used are all commercial products which are conventional in the art unless otherwise specified.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises, by mass, 10-20 parts of water-based epoxy resin, preferably 12-18 parts of water-based epoxy resin, and more preferably 15 parts of water-based epoxy resin. In the present invention, the aqueous epoxy resin preferably includes one or more of bisphenol a type epoxy resin, phenol type epoxy resin, and glycidyl ether type epoxy resin. In the present invention, the source of the aqueous epoxy resin is preferably from environmental protection technologies, ltd, virtue of south of Hunan.
The heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system comprises, by mass, 5-15 parts of hydrophilic carbon nanotubes, preferably 8-12 parts of hydrophilic carbon nanotubes, and more preferably 10 parts of hydrophilic carbon nanotubes. In the present invention, the particle size of the hydrophilic carbon nanotube is preferably 0.01 to 1 μm. The hydrophilic carbon nano tube has good heat conducting performance and heat transfer performance, the surface of the hydrophilic carbon nano tube also has hydroxyl, sulfonic group and a small amount of amino hydrophilic groups, the hydrophilic carbon nano tube has good hydrophilicity, and the dispersion in the heat-dissipating coating is high. In the invention, the contact area of the hydrophilic carbon nano tube chain structure and the hydrophilic kaolin layered structure in the aqueous epoxy resin is increased, and the two components generate synergistic action to form a perfect heat conducting network, so that the heat conducting property of the heat radiating coating of the aqueous carbon nano tube/epoxy resin dispersion system is effectively improved, and the reduction of the mechanical property can be reduced.
In the present invention, the hydrophilic carbon nanotube is preferably prepared by mixing carbon nanotube, anionic surfactant, phase transfer catalyst, dispersant and water, and performing a modification reaction.
In the present invention, the order of mixing the carbon nanotube, the anionic surfactant, the phase transfer catalyst, the dispersant and the water is preferably that the carbon nanotube, the anionic surfactant, the phase transfer catalyst and part of the water are first mixed to obtain a carbon nanotube mixed solution; secondly, mixing the dispersant and the residual water to obtain a dispersant water solution; and carrying out third mixing on the carbon nano tube mixed solution and the dispersant aqueous solution, and carrying out modification reaction to obtain the hydrophilic carbon nano tube. In the present invention, the first mixing mode is preferably magnetic stirring, and the rotation speed and time of the magnetic stirring are not particularly limited in the present invention, and the raw materials may be dissolved. In the present invention, the temperature of the first mixing is preferably 40 to 50 ℃. In the present invention, the second mixing mode is preferably magnetic stirring, and the rotation speed and time of the magnetic stirring are not particularly limited in the present invention, and the raw materials may be dissolved. In the present invention, the temperature of the second mixing is preferably 90 to 100 ℃. In the present invention, the third mixing mode is preferably magnetic stirring; the magnetic stirring time is preferably 1-3 h. The rotation speed of the magnetic stirring is not specially limited, and the raw materials can be uniformly dispersed. In the invention, the mass ratio of the carbon nanotube, the anionic surfactant, the phase transfer catalyst and the dispersing agent is preferably (1-2): (1-2): (0.5-1): (3-5), more preferably (1.2-1.8): (1.2-1.8): (0.6-0.8): (3.3-4.5). In the present invention, the water is preferably distilled water. In the present invention, the volume ratio of the partial water to the remaining water is preferably 1: 2.
in the present invention, the anionic surfactant preferably includes one or more of sodium lauryl sulfate, sodium dodecylbenzenesulfonate and sodium hexadecylsulfonate. In the preparation process of the hydrophilic carbon nano tube, an anionic surfactant wraps the outer surface of the carbon nano tube and is ionized simultaneously to generate hydrophilic group ether sulfonic acid group, the ether sulfonic acid group and oxygen-containing functional groups on the surface of the carbon nano tube are subjected to modification reaction to generate hydroxyl, sulfonic acid group and a small amount of amino hydrophilic groups, the hydrophilicity of the carbon nano tube is enhanced, and the hydrophilic carbon nano tube is obtained and forms a uniform and stable dispersion system in the water-based epoxy resin.
In the present invention, the dispersant preferably includes polyvinyl alcohol and/or polyethylene glycol. In the preparation process of the hydrophilic carbon nano tube, the dispersant can improve the hydrophilicity of the carbon nano tube, so that the dispersibility of the hydrophilic carbon nano tube in the aqueous epoxy resin is improved.
In the present invention, the phase transfer catalyst preferably comprises one or more of tetrabutylammonium bromide (TBAB), triethylbenzylammonium bromide (TEBA) and cetyltrimethylammonium bromide (CTMAB). In the preparation process of the hydrophilic carbon nano tube, the phase transfer catalyst can effectively promote the wetting and dissolving of the carbon nano tube in the aqueous solution and improve the dispersibility of the hydrophilic carbon nano tube in the aqueous epoxy resin.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises, by mass, 5-20 parts of hydrophilic kaolin, preferably 8-15 parts of hydrophilic kaolin, and more preferably 10-12 parts of hydrophilic kaolin. In the invention, the hydrophilic kaolin has excellent bonding property, mechanical property and heat conduction property, the surface of the hydrophilic kaolin also has hydroxyl, sulfonic group and a small amount of amino hydrophilic groups, the hydrophilic kaolin has good hydrophilicity and high dispersibility in the heat dissipation coating.
In the present invention, the hydrophilic kaolin is preferably prepared by mixing calcined kaolin, an anionic surfactant, a phase transfer catalyst, a dispersant and water, and performing a modification reaction.
In the present invention, the calcined kaolin, the anionic surfactant, the phase transfer catalyst, the dispersant and water are preferably mixed in this order by first mixing the calcined kaolin, the anionic surfactant, the phase transfer catalyst and part of the water to obtain a kaolin mixed solution; secondly, mixing the dispersant and the residual water to obtain a dispersant water solution; and carrying out third mixing on the kaolin mixed solution and a dispersant aqueous solution, and carrying out modification reaction to obtain the hydrophilic kaolin. In the present invention, the first mixing mode is preferably magnetic stirring, and the rotation speed and time of the magnetic stirring are not particularly limited in the present invention, and the raw materials may be dissolved. In the present invention, the temperature of the first mixing is preferably 40 to 50 ℃. In the present invention, the second mixing mode is preferably magnetic stirring, and the rotation speed and time of the magnetic stirring are not particularly limited in the present invention, and the raw materials may be dissolved. In the present invention, the temperature of the second mixing is preferably 90 to 100 ℃. In the present invention, the third mixing mode is preferably magnetic stirring; the magnetic stirring time is preferably 1-3 h. The rotation speed of the magnetic stirring is not specially limited, and the raw materials can be uniformly dispersed.
In the invention, the mass ratio of the calcined kaolin, the anionic surfactant, the phase transfer catalyst and the dispersing agent is preferably (1-2): (1-2): (0.5-1): (3-5), more preferably (1.2-1.8): (1.2-1.8): (0.6-0.8): (3.3-4.5). In the present invention, the water is preferably distilled water. In the invention, the volume ratio of the partial water to the residual water is preferably 2-3: 5-9. In the invention, the particle size of the hydrophilic kaolin is preferably 0.01-1 μm. The calcined kaolin has a disordered metakaolin structure, so that partial groups of the inner layer of the original crystal are exposed, the types and the number of surface active points are increased, and the reaction activity is high.
In the present invention, the anionic surfactant preferably includes one or more of sodium lauryl sulfate, sodium dodecylbenzenesulfonate and sodium hexadecylsulfonate. In the preparation process of the hydrophilic kaolin, an anionic surfactant wraps the outer surface of the kaolin and is ionized simultaneously to generate a hydrophilic group ether sulfonic group, the ether sulfonic group and an oxygen-containing functional group on the surface of the kaolin are subjected to modification reaction to generate a hydroxyl group, a sulfonic group and a small amount of amine groups, the hydrophilicity of the kaolin is enhanced, and the hydrophilic kaolin is obtained and forms a uniform and stable dispersion system in the waterborne epoxy resin.
In the present invention, the dispersant preferably includes polyvinyl alcohol and/or polyethylene glycol. In the preparation process of the hydrophilic kaolin, the dispersant can improve the hydrophilicity of the kaolin, so that the dispersibility of the hydrophilic kaolin in the aqueous epoxy resin is improved.
In the present invention, the phase transfer catalyst preferably comprises one or more of tetrabutylammonium bromide (TBAB), triethylbenzylammonium bromide (TEBA) and cetyltrimethylammonium bromide (CTMAB). In the preparation process of the hydrophilic kaolin, the phase transfer catalyst can effectively promote the wetting and dissolving of the kaolin in the aqueous solution, and improve the dispersibility of the hydrophilic kaolin in the aqueous epoxy resin.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises 1-5 parts by mass of an antifoaming agent, preferably 2-4 parts by mass, and more preferably 3 parts by mass of a water-based epoxy resin. In the present invention, the defoaming agent preferably includes one or more of tributyl phosphate, polyether-based defoaming agents, and silicone defoaming agents.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises, by mass, 1-5 parts of a leveling agent, preferably 2-4 parts, and more preferably 3 parts. In the present invention, the leveling agent includes one or more of a polyurethane leveling agent, an organosilicon leveling agent, and an acrylic leveling agent.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises 3-10 parts by mass of a two-component water-based epoxy resin curing agent, preferably 5-8 parts by mass, and more preferably 6 parts by mass. In the invention, the two-component water-based epoxy resin curing agent is preferably selected from the environmental protection science and technology limited of Hunan virtue.
The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system comprises 0-10 parts of water, preferably 1-5 parts of water, and more preferably 3 parts of water by mass; the water is preferably distilled water.
In the invention, the solid content of the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system is preferably 55-75%.
The invention also provides a preparation method of the heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system, which comprises the following steps:
and sequentially mixing the water-based epoxy resin, the hydrophilic carbon nano tube, the hydrophilic kaolin, water, the defoaming agent, the leveling agent and the double-component water-based epoxy curing agent to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
In the present invention, the mixing method is preferably magnetic stirring, and the rotation speed and time of the magnetic stirring are not particularly limited in the present invention, and the raw materials may be uniformly mixed. In the invention, the mixing sequence can ensure that the hydrophilic carbon nano tube and the hydrophilic kaolin are fully contacted with the epoxy resin, and the dispersibility of the hydrophilic carbon nano tube and the hydrophilic kaolin in the epoxy resin is improved.
The invention also provides the application of the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system in the technical scheme or the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system prepared by the preparation method in the technical scheme in a metal heat-dissipating product.
The invention also provides the application of the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system in the technical scheme or the heat-dissipating coating of the water-based carbon nanotube/epoxy resin dispersion system prepared by the preparation method in the technical scheme in metal corrosion prevention.
The application mode of the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system is not particularly limited, and can be any application mode known to those skilled in the art, such as brushing or coating. In the invention, the brushing amount is preferably 8-10 g/m2(ii) a The coating amount is preferably 10g/m2。
Before brushing or coating the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system, the invention preferably sequentially carries out oil removal, hot water washing, first flow washing, acid washing, second flow washing, surface conditioning, third flow washing, phosphating, recovery, fourth flow washing and drying on the metal surface.
According to the invention, the oil removing agent preferably comprises sodium hydroxide, sodium carbonate and an OP emulsifier, the mass volume ratio of the sodium hydroxide to the sodium carbonate to the OP emulsifier is preferably 5-10 g: 10-25 g: 15-20 m L, and the further preferred ratio is 8 g: 15-20 g: 18m L, in the invention, the oil removing temperature is preferably 50-60 ℃, the oil removing time is preferably 2-4 min, and in the invention, the metal is preferably soaked in an oil removing agent for oil removing.
In the present invention, the hot water temperature of the hot water washing is preferably 90 ℃.
In the present invention, the water flow rates of the first, second, third and fourth water washes are independently preferably 1 m/s.
In the present invention, the acid washing reagent is preferably a hydrochloric acid solution having a mass concentration of 10% to 25%. In the invention, the pickling temperature is preferably 40-50 ℃; the pickling time is preferably 0.5-1 min.
In the present invention, the reagent for surface modification is preferably an oxalic acid solution having a mass concentration of 2% to 4%. In the invention, the temperature of the surface adjustment is preferably 20-25 ℃; the time for the surface adjustment is preferably 0.5-1 min. The invention improves the efficiency of subsequent phosphating treatment by surface adjustment, so that fine phosphating crystallization is realized and the phosphating quality is improved.
In the present invention, the phosphating agent is preferably prepared by mixing the following raw materials: zinc nitrate solution, nickel nitrate solution, zinc phosphate solution and tartaric acid solution. In the invention, the mass ratio of zinc nitrate in the zinc nitrate solution, nickel nitrate in the nickel nitrate solution, zinc phosphate in the zinc phosphate solution and tartaric acid in the tartaric acid solution is preferably (85-90): (2-5): (50-55): (0.5 to 1), and more preferably 87: 3: 53: 0.8. in the invention, the temperature of the phosphorization is preferably 50-53 ℃; the time for phosphorization is preferably 5-15 min. The invention improves the binding force between the metal surface and the coating through phosphating treatment and improves the corrosion resistance.
The following will describe the heat-dissipating coating material of the aqueous carbon nanotube/epoxy resin dispersion system and the preparation method and application thereof in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Weighing 1g of carbon nano tube in a beaker, then weighing 2g of lauryl sodium sulfate, 0.5g of tetrabutyl ammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water, and carrying out magnetic stirring to obtain the hydrophilic carbon nano tube;
weighing 1g of calcined kaolin in a beaker, and then weighing 2g of sodium dodecyl sulfate, 0.5g of tetrabutylammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water for magnetic stirring to obtain hydrophilic kaolin;
weighing 15g of water-based epoxy resin, 8g of hydrophilic carbon nano tube, 12g of hydrophilic kaolin and 3g of water in a beaker, uniformly stirring, weighing 1g of tributyl phosphate, 1g of polyurethane flatting agent and 3g of double-component water-based epoxy curing agent, and stirring for 2h by using a DW-2 force-increasing stepless constant-speed stirrer until the mixture is uniformly dispersed to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
Degreasing the surface of a 12cm × 5cm galvanized steel plate in sequence (the mass-volume ratio of sodium hydroxide, sodium carbonate and OP emulsifier in a degreasing agent is 10 g: 25 g: 20m L, the temperature is 60 ℃, the time is 4min), hot water washing (the temperature of hot water is 90 ℃, the flow rate is 1m/s), first washing (the flow rate is 1m/s), acid washing (the acid washing agent is 25% hydrochloric acid solution, the temperature is 50 ℃, the time is 1min), second washing (the flow rate is 1m/s), surface conditioning (the surface conditioning agent is 4% oxalic acid solution, the temperature is 25 ℃, the time is 1min), third washing (the flow rate is 1m/s), phosphating (the mass ratio of zinc nitrate in a zinc nitrate solution in a phosphating agent, nickel nitrate in a nickel nitrate solution, zinc phosphate in a zinc phosphate solution and tartaric acid in a tartaric acid solution is 90: 5: 55: 1, the temperature is 53 ℃, the time is 15min), recovering, fourth washing (the flow rate is 1m/s) and drying, then the water-based on the surface of the nano-tube coating system is coated on the heat dissipation resin, the water-based on the coating system, the water-based on the mass-based on the zinc oxide coating, the water-based on the mass-based on the coating, the heat-resistant coating system, the heat-resistant coating2(ii) a And applied to the surface of 1 glass plate to measure the hardness of the coating pendulum, the coating amount applied to the surface of the glass plate being 3g/m2After drying in an oven at 50 ℃, water-based epoxy resin coatings, respectively designated as a1, a2, A3, a4 and B1, were obtained, and the adhesion, impact resistance, flexibility, salt spray resistance and pendulum hardness of the coatings were respectively tested, and the test results are shown in table 1.
The heat conductivity of the heat-dissipating coating of the obtained water-based carbon nanotube/epoxy resin dispersion system is tested, and the heat conductivity test method comprises the following steps:
(1) four 100 × 100 carbon steel plates of 100 mm 100 × 1mm are selected, one plate is not coated with any paint and is used as a comparison sample A, one plate is coated with a layer of red alkyd resin, the half area of the surface of the obtained red alkyd resin coating is coated with the heat dissipation paint (hereinafter referred to as heat dissipation paint) of the aqueous carbon nano tube/epoxy resin dispersion system prepared in the example 1, which is recorded as B, one plate is coated with a layer of gray polyurethane paint, the half area of the surface of the obtained polyurethane paint film is coated with the heat dissipation paint, which is recorded as C, and one plate is coated with only the heat dissipation paint, which is recorded as D, the paint is coated by adopting a brush coating method, the thickness of each coating is 60 mu m, the paint is put into an oven to be dried at the temperature of 40 ℃, and the paint.
(2) The test piece is stuck to a probe of a temperature recorder, the test piece is placed on an electric hot plate, the temperature of the electric hot plate is set to be 90 ℃, the test piece is heated to be stabilized at 90 ℃, an infrared temperature measuring gun is used for measuring the infrared radiation temperature of the sides, covered with the heat dissipation coating, of the test piece B and the test piece C, and the temperature value is recorded; the test piece is rapidly transferred into a heat insulation box, when the test piece is cooled to below 40 ℃ in the box through heat dissipation, the temperature-lowering process and time are recorded through a temperature recorder, and a temperature-lowering curve is formed.
Comparing the cooling curves of different test pieces, if the test piece is cooled from 90 ℃ to 40 ℃ in a shorter time, the stronger the heat dissipation performance is, and the slope of the heat dissipation curve is large.
When the actual temperature of the test piece is stabilized at 90 ℃, an infrared temperature gun with EMS (infrared radiation coefficient) set as a fixed value is aligned to one side of the test piece B and one side of the test piece C, which are coated with the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system prepared by the invention, to measure the infrared temperature value, and the test piece with higher radiation coefficient can record a higher temperature measurement value due to stronger infrared radiation, thereby comparing the infrared radiation capability of different coatings at the same temperature. The stronger the infrared radiation capability is, the better the radiation heat dissipation and cooling performance can be considered.
FIG. 1 is a thermal conductivity chart of the thermal dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion prepared in example 1, wherein A is a thermal conductivity curve of a test piece A; b is a heat conductivity coefficient test curve of the test piece B; c is a heat conductivity coefficient test curve of the test piece C; d is the heat conductivity coefficient test curve of the test piece D. As can be seen from fig. 1: the heat-dissipating coating coated on the alkyd resin or polyurethane paint enhances the heat-conducting property of the steel plate; the steel plate coated with the heat dissipation coating only has enhanced heat conduction performance compared with the uncoated steel plate. The alkyd resin or polyurethane paint is used as the steel plate primer, and the function of the heat dissipation coating is not influenced. The heat-dissipation coating of the aqueous carbon nano tube/epoxy resin dispersion system prepared by the invention has good heat-conduction performance, can be fused with various commercially available primers, and has different heat-conduction performance according to different types of primers and different effects.
The heat dissipation performance of the heat dissipation coating of the water-based carbon nano tube/epoxy resin dispersion system is tested by adopting a hemisphere emissivity tester SK-B L C50, and the heat dissipation performance is tested by adopting an IC200 heat dissipation aluminum sheet, coating the heat dissipation coating according to GB/T4653-1984 general technical conditions for infrared radiation coatings, and testing the heat dissipation performance, wherein the test results are shown in Table 2.
Fig. 2 is a relative radiation energy spectrum of the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system prepared in example 1, and as can be seen from an analysis combining fig. 2 and table 2, when the normal total emissivity is greater than or equal to 0.85, the coating is qualified, and the normal total emissivity of the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system provided by the invention is 0.89, which is better than the standard value.
Comparative example 1
The commercially available imported similar oily system product (hong Kong constant light applied materials Co., Ltd.) was used as a comparative example, the coating was applied to the surface of a galvanized steel sheet in an amount of 2g, and after drying at 50 ℃ in an oven, a coating was obtained and was designated as D1, and the properties of the coating were measured, and the test results are shown in Table 1.
The heat dissipation performance of the paint was tested, and the test results are shown in table 2, and the test method was the same as that of example 1.
TABLE 1 results of the performance tests of A1, A2, A3, A4, B1 prepared in example 1 and D1 coating prepared in comparative example 1
According to the analysis of the experimental results, the conventional similar oily system product in the prior art of the heat dissipation coating adhesive of the water-based carbon nanotube/epoxy resin dispersion system has good salt spray resistance and good paint film performance. Compared with the conventional similar oily system product raw materials in the prior art, the raw materials of the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system prepared by the invention are more environment-friendly, and the discharge amount of VOC is less.
Example 2
This example differs from example 1 in the amount of starting material used.
Weighing 1g of carbon nano tube in a beaker, then weighing 2g of lauryl sodium sulfate, 0.5g of tetrabutyl ammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water, and carrying out magnetic stirring to obtain the hydrophilic carbon nano tube;
weighing 1g of calcined kaolin in a beaker, and then weighing 2g of sodium dodecyl sulfate, 0.5g of tetrabutylammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water for magnetic stirring to obtain hydrophilic kaolin;
weighing 15g of water-based epoxy resin, 10g of hydrophilic carbon nano tube, 12g of hydrophilic kaolin and 3g of water in a beaker, uniformly stirring, weighing 1g of tributyl phosphate, 1g of polyurethane leveling agent and 3g of double-component water-based epoxy curing agent, and stirring for 2h by using a DW-2 force-increasing stepless constant-speed stirrer until the mixture is uniformly dispersed to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
The heat dissipation performance of the obtained heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system was tested, the test results are shown in table 2, and the test method is the same as that of example 1.
Example 3
This example differs from example 1 in the amount of starting material used.
Weighing 1g of carbon nano tube in a beaker, then weighing 2g of lauryl sodium sulfate, 0.5g of tetrabutyl ammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water, and carrying out magnetic stirring to obtain the hydrophilic carbon nano tube;
weighing 1g of calcined kaolin in a beaker, and then weighing 2g of sodium dodecyl sulfate, 0.5g of tetrabutylammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water for magnetic stirring to obtain hydrophilic kaolin;
weighing 15g of water-based epoxy resin, 12g of hydrophilic carbon nano tube, 0.5g of hydrophilic kaolin and 3g of water in a beaker, uniformly stirring, weighing 1g of tributyl phosphate, 1g of polyurethane leveling agent and 3g of double-component water-based epoxy curing agent, and stirring for 2h by using a DW-2 force-increasing stepless constant-speed stirrer until the mixture is uniformly dispersed to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
The heat dissipation performance of the obtained heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system was tested, the test results are shown in table 2, and the test method is the same as that of example 1.
Comparative example 2
This comparative example differs from example 1 in the amount of raw materials used for the heat-dissipating coating of the aqueous carbon nanotube/epoxy dispersion.
Weighing 1g of carbon nano tube in a beaker, then weighing 2g of lauryl sodium sulfate, 0.5g of tetrabutyl ammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water, and carrying out magnetic stirring to obtain the hydrophilic carbon nano tube;
weighing 1g of calcined kaolin in a beaker, and then weighing 2g of sodium dodecyl sulfate, 0.5g of tetrabutylammonium bromide, 3g of polyvinyl alcohol and 45m of L distilled water for magnetic stirring to obtain hydrophilic kaolin;
weighing 20g of water-based epoxy resin, 8g of hydrophilic carbon nano tube, 12g of hydrophilic kaolin and 3g of water in a beaker, uniformly stirring, weighing 1g of tributyl phosphate, 1g of polyurethane flatting agent and 3g of double-component water-based epoxy curing agent, and stirring for 2h by using a DW-2 force-increasing stepless constant-speed stirrer until the mixture is uniformly dispersed to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
The heat dissipation performance of the obtained heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system was tested, the test results are shown in table 2, and the test method is the same as that of example 1.
TABLE 2 Heat dissipation Performance test results for coatings prepared in examples 1 to 3 and comparative examples 1 to 2
| Detecting items | Technical index | The result of the detection | Singleton decision |
| Example 1 | ≥0.85 | 0.89 | Conform to |
| Example 2 | ≥0.85 | 0.89 | Conform to |
| Example 3 | ≥0.85 | 0.89 | Conform to |
| Comparative example 1 | ≥0.85 | 0.89 | Conform to |
| Comparative example 2 | ≥0.85 | 0.89 | Conform to |
According to the analysis of the experimental results, the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system provided by the invention has better heat dissipation performance than the conventional similar oily system products in the prior art, and the raw materials of the heat dissipation coating of the aqueous carbon nanotube/epoxy resin dispersion system prepared by the invention are more environment-friendly and have less discharge of VOC compared with the conventional similar oily system products in the prior art.
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. The heat dissipation coating of the water-based carbon nanotube/epoxy resin dispersion system is characterized by comprising the following components in parts by mass:
10-20 parts of water-based epoxy resin, 5-15 parts of hydrophilic carbon nano tubes, 5-20 parts of hydrophilic kaolin, 0-10 parts of water, 1-5 parts of defoaming agent, 1-5 parts of flatting agent and 3-10 parts of two-component water-based epoxy resin curing agent.
2. The heat-dissipating coating material of an aqueous carbon nanotube/epoxy resin dispersion system according to claim 1, wherein the hydrophilic carbon nanotube is prepared by mixing raw materials including a carbon nanotube, an anionic surfactant, a phase transfer catalyst, a dispersant and water, and performing a modification reaction;
the mass ratio of the carbon nano tube, the anionic surfactant, the phase transfer catalyst and the dispersing agent is (1-2): (1-2): (0.5-1): (3-5).
3. The heat-dissipating coating material of an aqueous carbon nanotube/epoxy resin dispersion system according to claim 1 or 2, wherein the hydrophilic carbon nanotubes have a particle size of 0.01 to 1 μm.
4. The heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system according to claim 1, wherein the hydrophilic kaolin is prepared by mixing calcined kaolin, an anionic surfactant, a phase transfer catalyst, a dispersant and water, and performing a modification reaction;
the mass ratio of the calcined kaolin to the anionic surfactant to the phase transfer catalyst to the dispersant is (1-2): (1-2): (0.5-1): (3-5).
5. The heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system according to claim 1 or 4, wherein the hydrophilic kaolin has a particle size of 0.01 to 1 μm.
6. The heat-dissipating coating of an aqueous carbon nanotube/epoxy dispersion according to claim 1, wherein the aqueous epoxy resin preferably comprises one or more of bisphenol a type epoxy resin, novolac type epoxy resin, and glycidyl ether type epoxy resin.
7. The thermal dissipation coating of aqueous carbon nanotube/epoxy dispersion system according to claim 1, wherein the defoamer comprises one or more of tributyl phosphate, polyether defoamer and silicone defoamer.
8. The aqueous carbon nanotube/epoxy dispersion heat-dissipating coating according to claim 1, wherein the leveling agent comprises one or more of a polyurethane leveling agent, an organosilicon leveling agent, and an acrylic leveling agent.
9. The method for preparing the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion system according to any one of claims 1 to 8, comprising the steps of:
and sequentially mixing the water-based epoxy resin, the hydrophilic carbon nano tube, the hydrophilic kaolin, water, the defoaming agent, the leveling agent and the double-component water-based epoxy curing agent to obtain the heat-dissipating coating of the water-based carbon nano tube/epoxy resin dispersion system.
10. Use of the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion according to any one of claims 1 to 8 or the heat-dissipating coating of the aqueous carbon nanotube/epoxy resin dispersion prepared by the preparation method according to claim 9 in a metal heat-dissipating product.
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