CN109554071B - Titanium dioxide nano-carbon composite static conductive heat dissipation coating and preparation method thereof - Google Patents
Titanium dioxide nano-carbon composite static conductive heat dissipation coating and preparation method thereof Download PDFInfo
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- CN109554071B CN109554071B CN201811380651.2A CN201811380651A CN109554071B CN 109554071 B CN109554071 B CN 109554071B CN 201811380651 A CN201811380651 A CN 201811380651A CN 109554071 B CN109554071 B CN 109554071B
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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
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting 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
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2241—Titanium dioxide
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a titanium dioxide nanocarbon composite static conductive heat dissipation coating and a preparation method thereof. The coating comprises the following raw materials in parts by weight: 30-50 parts of epoxy resin; 10-30 parts of curing agent; 30-50 parts of isobutyl titanate; 3-10 parts of carbon nano tubes; 5-10 parts of mica powder; 1-3 parts of fumed silica; 1-10 parts of nano dispersant; 0.1-1 parts of leveling agent; 0.1-0.5% of defoaming agent; 30-50 parts of dimethylbenzene; 30-50 parts of n-butyl alcohol; 30-50 parts of isopropanol; 0.3-1.5 of divinyl triamine; 10-20 parts of butyl acetate; 80-100 parts of distilled water. According to the invention, the titanium dioxide nanosheets are grown in situ on the surfaces of the carbon nanotubes, so that the dispersibility of the nanocarbon filler in the coating and the compatibility with resin are better, the product has no pollution to oil products, and the product has excellent comprehensive performances of good conductivity, oil resistance, water resistance, high temperature resistance, corrosion resistance, ageing resistance, high adhesion, good heat dissipation performance and the like.
Description
Technical Field
The invention relates to the field of coatings, in particular to a titanium dioxide nanocarbon composite static conductive heat dissipation coating and a preparation method thereof.
Background
With the development of science and technology, various polymer synthetic materials are continuously emerged and are applied in a large amount in the life and production of people, so that the life and production quality of people are greatly improved; however, most of the polymer materials have poor electrical conductivity, and therefore, static electricity is easily accumulated during use, and the damage caused by the static electricity is increasingly highlighted, and meanwhile, a large amount of heat is generated. In recent years, numerous accidents have been caused by static electricity interference and damage (such as causing misoperation of electronic and electric equipment), and a great economic loss is caused. Therefore, in order to eliminate the influence of static electricity and temperature rise, it is necessary to use the static electricity conductive heat dissipation coating in proper occasions.
The static electricity conducting and heat dissipating coating is a coating material with wide application, integrates the double advantages of static electricity conducting and heat dissipating, can not only lead out static charges accumulated on the surface of the material and eliminate the static electricity, but also play a role in heat dissipating, and is suitable for more coating fields.
The current static conductive heat dissipation coating mainly comprises three types: one type is mainly carbon black or conductive fiber, and in the using process, the carbon black and the conductive fiber are easily extracted, so that oil products can be polluted, and meanwhile, the adhesive force and the corrosion resistance are not ideal; the other is that metal or metal oxide is used as a conductive functional body, when the metal or the metal oxide is used as the conductive functional body, the metal is easy to be oxidized, and the conductive performance is unstable; the third type is a mixture of a carbon material and a metal oxide, etc., and the problem of dispersion is prominent, and the two former problems remain.
At present, the single-function coating is more, and the multifunctional coating is scarce. The main problem of the static conductive coating used at present is poor compatibility of the conductive functional body and resin; the metal conductive functional body is easy to precipitate and has poor dispersibility; the conductivity of the semiconductor oxide conductive functional body is poor; the traditional carbon black has general conductivity, is easy to pollute oil products and cannot well meet the use requirements. In addition, the dispersion process of the carbon material is complex, the carbon material is easy to agglomerate, the carbon material and the resin have poor compatibility, and the combination is not tight. Meanwhile, the nano-fillers are various in types, and cannot be connected into an electric and heat conducting network inside, so that the direct synergistic effect of the nano-materials is poor and cannot be exerted.
Therefore, there is a need to provide a static conductive heat dissipation coating with good compatibility between the conductive functional body and the resin, good dispersibility of the conductive functional body, high conductivity and no pollution to the oil product, and a preparation method thereof.
Disclosure of Invention
In view of this, the invention provides a titanium dioxide nanocarbon composite static conductive heat dissipation coating and a preparation method thereof. The method of the invention has the following characteristics: (1) the titanium dioxide grows on the carbon nano tube in situ to prepare the composite material which is tightly connected, so that the situation that different nano materials cannot be connected and the synergistic effect is exerted is avoided; (2) titanium acid ester which is a precursor of titanium dioxide is used for growing on the surface of the carbon nano tube, so that the problem of agglomeration of the carbon nano tube is avoided, and the problem of agglomeration caused by directly adding titanium dioxide is also avoided; (3) the wetting property of the surface of the carbon material and the resin is poor, so that the carbon material and the resin are not tightly combined, the overall performance of the coating is influenced, and the problem of poor combination of the carbon material directly contacting the resin is solved through surface growth. The product prepared by the method has the advantages of good compatibility of the conductive functional body and resin, good dispersibility of the conductive functional body, no pollution to oil products, good conductivity, oil resistance, water resistance, high temperature resistance, corrosion resistance, ageing resistance, high adhesive force, good heat dissipation performance and other excellent comprehensive performances.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a titanium dioxide nanocarbon composite static conductive heat dissipation coating which comprises the following raw materials in parts by weight:
30-50 parts of epoxy resin; 10-30 parts of a curing agent; 30-50 parts of titanate; 3-10 parts of carbon nanotubes; 5-10 parts of mica powder; 1-3 parts of fumed silica; 1-10 parts of a nano dispersant; 0.1-1 part of a leveling agent; 0.1-0.5 part of defoaming agent; 30-50 parts of dimethylbenzene; 30-50 parts of n-butyl alcohol; 30-50 parts of isopropanol; 0.3-1.5 parts of divinyl triamine; 10-20 parts of butyl acetate; 80-100 parts of distilled water.
Preferably, the particle size of the coating is 3-5 um.
The epoxy resin is used as a binder (film-forming agent) of the coating, so that the filler can be dispersed in the resin and bonded to the surface of a coated object, and good mechanical properties, heat resistance and other properties are kept. Preferably, the epoxy resin is fluorine modified epoxy resin, and specifically, the epoxy resin can be fluorine modified epoxy resin E-20 or epoxy resin E-44 or a mixture of the two. Preferably, the epoxy resin is 40 parts by weight.
The curing agent is used for causing the epoxy resin to generate polymerization reaction and is an amine curing agent or an anhydride curing agent, so that the coating is cured to form a film. The curing agent used in the examples of the present invention is curing agent T-31, and the selection of the curing agent in the present invention is not limited. Preferably, the curing agent is 20 parts by weight.
The titanate serves to provide a titanium source, is a precursor of titanium dioxide, and decomposes into titanium dioxide under specific conditions. Preferably, the weight part of the titanate is 40 parts. Preferably, the titanate is an isopropyl titanate, an isopropyl titanate or a tetra-n-butyl titanate. The carbon nano tube has the function of utilizing the high conductivity and high thermal radiation coefficient of the carbon nano tube, and meanwhile, the nano tube is dispersed and presents network connection, so that the coating has a good internal conductive network and a good heat conductive network, and the electrostatic heat radiation function is exerted. Preferably, the carbon nanotube is a multi-walled carbon nanotube with a diameter of 10-100 nm. Preferably, the carbon nanotube is 8 parts by weight.
The mica powder has good heat radiation performance, improves the abrasion resistance and hardness of a paint film, and has good ultraviolet aging resistance and corrosion resistance. Preferably, the mica powder is 6 parts by weight.
The fumed silica is used as an anti-settling agent and a thickening agent to adjust the dispersion problem of the filler in the coating, which is beneficial to grinding the coating, so that the coating keeps a certain viscosity, and the water resistance of a paint film is improved. Preferably, the fumed silica is present in an amount of 2 parts by weight.
The function of the nano dispersant is to improve the surface wetting property of the nano filler and help the dispersion of the filler in the resin. The nano dispersant of the embodiment of the invention is selected from Diperbyk-163 of Germany. Preferably, the nano dispersant is 5 parts by weight.
The leveling agent can promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process. The leveling agent of the present embodiment is selected from BYK-410, bib, germany. Preferably, the leveling agent is 0.5 part by weight.
The defoaming agent functions to eliminate bubbles of the coating. The defoaming agent of the present embodiment is selected from German Bike BKY-052. Preferably, the defoamer is present in an amount of 0.2 parts by weight.
Xylene is a constituent of paint diluents, regulating the solubility and polarity of the diluent. Preferably, the xylene is 50 parts by weight.
N-butanol is a component of the paint diluent, regulating the solubility and polarity of the diluent. Preferably, the weight part of the n-butanol is 30 parts.
Isopropanol serves as a dispersion solvent for the carbon nanotubes and a diluent for the divinyltriamine. Preferably, the weight part of the isopropyl alcohol is 40 parts.
The divinyl triamine has the function of inhibiting the titanate from hydrolysis, so that the titanate is slowly hydrolyzed to generate the nano titanium dioxide. Preferably, the weight part of the divinyltriamine is 1 part.
Butyl acetate is a component of the paint diluent, regulating the solubility and polarity of the diluent. Preferably, the butyl acetate is 20 parts by weight.
Distilled water is the solvent for the hydrolysis of titanate to titanium dioxide. Preferably, the distilled water is 80 parts by weight.
The invention also provides a preparation method of the titanium dioxide nanocarbon composite static conductive heat dissipation coating, which comprises the following steps:
(1) dispersing carbon nano tubes in isopropanol solution, adding divinyl triamine and uniformly stirring;
(2) adding titanate into the solution obtained in the step (1), uniformly stirring, and adding distilled water for dilution;
(3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction to obtain a composite conductive film solution;
(4) performing centrifugal operation on the composite conductive film solution obtained in the step (3), and drying the solid to obtain a composite nano filler;
(5) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion to obtain a premix A;
(6) adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B;
(7) physically mixing the premix A and the premix B to obtain a mixed material;
(8) grinding the mixed material obtained in the step (7) in a three-roller machine to obtain the titanium dioxide nano carbon composite static conductive and heat dissipation coating; taking out, sealing, bottling and storing;
(9) when in use, the curing agent is added into the components in the step (8) according to the proportion, and the coating operation can be carried out after the curing agent is uniformly stirred.
The steps are described in detail below:
and (1) dispersing the carbon nano tubes in an isopropanol solution, adding divinyl triamine into the isopropanol solution, and uniformly stirring.
Wherein, the weight part of the carbon nano tube is 3 to 10 parts, and the preferential part is 8 parts. The carbon nano tube is a multi-wall carbon nano tube, and the diameter of the carbon nano tube is 10-100 nm. The coating has the advantages that the high conductivity and high thermal radiation coefficient of the carbon nano tubes are utilized, and meanwhile, the nano tubes are dispersed and form network connection, so that the coating has a good internal conductive network and a good thermal conductive network, and the electrostatic conductive thermal radiation function is played.
The weight portion of the isopropanol is 30-50 parts, and preferably 40 parts. The isopropanol serves as a dispersion solvent of the carbon nano tube and also serves as a diluent of the diethyltriamine.
The weight part of the divinyl triamine is 0.3-1.5 parts, and preferably 1 part. The divinyl triamine has the function of inhibiting the titanate from hydrolysis, so that the titanate is slowly hydrolyzed to generate the nano titanium dioxide.
Preferably, the carbon nanotubes are dispersed in the isopropanol solution by ultrasound in the step (1), and the ultrasound time is preferably 0.5 h.
And (2) adding titanate into the solution obtained in the step (1), uniformly stirring, and adding distilled water for dilution.
Wherein, the weight portion of the titanate is 30 to 50 portions, preferably 40 portions. The titanate serves to provide a titanium source, is a precursor of titanium dioxide, and decomposes into titanium dioxide under specific conditions.
The weight portion of the distilled water is 80-100 portions, preferably 80 portions. Distilled water is the solvent for the hydrolysis of titanate to titanium dioxide.
And (3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction to obtain a composite conductive film solution.
The hydrothermal reaction realizes in-situ growth of the titanium dioxide nanosheet on the surface of the carbon nanotube to form a composite conductive film solution similar to a sandwich structure. The sandwich structure is a three-dimensional nano composite structure; the middle of the sandwich structure is a carbon nano tube, and the outside of the sandwich structure is a three-dimensional nano composite structure. The middle of the sandwich structure is a carbon nano tube, and the outside is coated with titanium dioxide.
Preferably, the temperature of the hydrothermal reaction in the step (3) is 200-250 ℃ and the time is 24-26 h.
And (4) carrying out centrifugal operation on the composite conductive filler solution obtained in the step (3), and drying the solid to obtain the composite nano filler.
And centrifuging to remove the solvent to obtain a solid, namely the titanium dioxide nano carbon sandwich structure composite nano filler growing in situ.
Preferably, the drying in step (4) is vacuum drying at 60-80 ℃.
And (5) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion to obtain a premix A.
Wherein, the dimethylbenzene, the n-butyl alcohol and the butyl acetate are all composition components of the paint thinner, and the solubility and the polarity of the thinner are adjusted. And (4) carrying out ultrasonic dispersion to obtain the premix A with uniform mixing and dispersion.
Preferably, the time of the ultrasonic dispersion in the step (5) is 0.5-1 h.
And (6) adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B.
Wherein, the weight part of the epoxy resin is 30 to 50 parts, preferably 40 parts. The epoxy resin is used as a binder (film-forming agent) of the coating, so that the filler can be dispersed in the resin and bonded on the surface of a coated object, and good mechanical properties, heat resistance and other properties are kept. Preferably, the epoxy resin is a fluorine modified epoxy resin, and the epoxy resin is epoxy resin E-20 or epoxy resin E-44 or a mixture of the two.
The total weight parts of the xylene, the n-butanol and the butyl acetate solvent in the step (5) and the step (6) are respectively as follows: 30-50 parts, 30-50 parts and 10-20 parts. Preferably, the weight part of xylene is 50 parts; the weight portion of the n-butyl alcohol is 30 portions; the weight portion of butyl acetate is 20 portions.
And (7) physically mixing the premix A and the premix B to obtain a mixed material.
The mica powder has good heat radiation performance, abrasion resistance and hardness of a paint film are improved, and the mica powder has good ultraviolet aging resistance and corrosion resistance. Preferably, the mica powder is 6 parts by weight.
The fumed silica is used as an anti-settling agent and a thickening agent to adjust the dispersion problem of the filler in the coating, which is beneficial to grinding the coating, so that the coating keeps a certain viscosity, and the water resistance of a paint film is improved. Preferably, the fumed silica is present in an amount of 2 parts by weight.
The function of the nano dispersant is to improve the surface wetting property of the nano filler and help the dispersion of the filler in the resin. The nano dispersant of the embodiment of the invention is selected from Diperbyk-163 of Germany. Preferably, the nano dispersant is 5 parts by weight.
The leveling agent can promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process. The leveling agent of the present embodiment is selected from BYK-410, bib, germany. Preferably, the leveling agent is 0.5 part by weight.
The defoaming agent functions to eliminate bubbles of the coating. The defoaming agent of the present embodiment is selected from German Bike BKY-052. Preferably, the defoamer is present in an amount of 0.2 parts by weight.
Preferably, the physical mixing in step (7) comprises: and (3) putting the premix A, the premix B and all the rest components into a mixer, stirring at a high speed for 1-1.5 h, and physically mixing.
Step (8), grinding the mixed material obtained in the step (7) in a three-roller machine to obtain the titanium dioxide nano carbon composite static conductive and heat dissipation coating; taking out, sealing, bottling and storing.
The particle size of the ground coating is 3-5 μm. Preferably, the grinding time in the step (8) is 2-3 h.
When the curing agent is used in the step (9), the curing agent is added into the components in the step (8) according to the proportion, and the coating operation can be carried out after the curing agent is uniformly stirred.
The curing agent is used for causing the epoxy resin to generate polymerization reaction and is an amine curing agent or an anhydride curing agent, so that the coating is cured to form a film. The weight part of the curing agent is 10-30 parts; preferably 20 parts.
The invention has the following beneficial effects:
according to the invention, the titanium dioxide nanosheets are grown in situ on the surface of the carbon nanotube, so that the dispersibility of the nano carbon filler in the coating and the compatibility of the nano carbon filler with resin are better.
The invention adopts the titanium dioxide nano carbon sandwich composite nano filler which grows in situ as a conductive functional body, and combines an optimized coating preparation process to obtain the titanium dioxide nano carbon composite static conductive heat dissipation coating; the static conductive coating formed by the heat dissipation coating has excellent comprehensive performances of good conductivity, lasting oil resistance, water resistance, high temperature resistance, corrosion resistance, ageing resistance, high adhesion, good heat dissipation performance, no pollution to oil products, no influence on recycling of oil storage tanks and the like, and can meet the relevant requirements of GB6590-2001 light oil product safety static conductivity in an ultrahigh standard.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The nanometer dispersant in the embodiment of the invention is German Bick Disperbyk-163; the leveling agent is selected from German BYK-410; the defoaming agent is selected from German Bike BKY-052. Those skilled in the art can select the product model in the specific application process, and the invention is not limited thereto.
Example 1
This example prepares a titanium dioxide nanocarbon composite static conductive and heat dissipation coating. The used raw materials comprise the following components in parts by weight:
the preparation process comprises the following steps:
(1) dispersing the carbon nano tube in isopropanol solution, carrying out ultrasonic dispersion for 0.5h, adding divinyl triamine, and stirring uniformly.
(2) Adding isobutyl titanate into the solution obtained in the step (1), stirring uniformly, and adding distilled water for dilution.
(3) And (3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction, controlling the temperature of the hydrothermal reaction to be 200-250 ℃ and the time to be 24-26 h. And (3) growing the titanium dioxide nanosheet on the surface of the carbon nanotube in situ to form a composite conductive film solution similar to a sandwich structure.
(4) And (4) carrying out centrifugal operation on the composite conductive film solution obtained in the step (3), and carrying out vacuum drying at the temperature of 60-80 ℃ to obtain the composite nano filler.
(5) And (4) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion for 0.5-1 h to obtain a premix A.
(6) And adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B.
(7) And (4) putting the premix A obtained in the step (5) and the premix B obtained in the step (6) into a mixer, stirring at a high speed for 1-1.5 h, and physically mixing to obtain a mixed material.
(8) And (4) putting the mixed material obtained in the step (7) into a three-roller machine, grinding for 2-3 h, taking out, sealing and bottling to obtain the titanium dioxide nano-carbon composite static conductive and heat dissipation coating.
(9) When in use, the curing agent is added into the component in the step (8) according to the proportion, and the coating operation is carried out after the curing agent is uniformly stirred.
Example 2
This example prepares a titanium dioxide nanocarbon composite static conductive and heat dissipation coating. The used raw materials comprise the following components in parts by weight:
the preparation process comprises the following steps:
(1) dispersing the carbon nano tube in isopropanol solution, carrying out ultrasonic dispersion for 0.5h, adding divinyl triamine, and stirring uniformly.
(2) Adding isobutyl titanate into the solution obtained in the step (1), stirring uniformly, and adding distilled water for dilution.
(3) And (3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction, controlling the temperature of the hydrothermal reaction to be 200-250 ℃ and the time to be 24-26 h. And (3) growing the titanium dioxide nanosheet on the surface of the carbon nanotube in situ to form a composite conductive film solution similar to a sandwich structure.
(4) And (4) carrying out centrifugal operation on the composite conductive film solution obtained in the step (3), and carrying out vacuum drying at the temperature of 60-80 ℃ to obtain the composite nano filler.
(5) And (4) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion for 0.5-1 h to obtain a premix A.
(6) And adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B.
(7) And (4) putting the premix A obtained in the step (5) and the premix B obtained in the step (6) into a mixer, stirring at a high speed for 1-1.5 h, and physically mixing to obtain a mixed material.
(8) And (4) putting the mixed material obtained in the step (7) into a three-roller machine, grinding for 2-3 h, taking out, sealing and bottling to obtain the titanium dioxide nano-carbon composite static conductive and heat dissipation coating.
(9) When in use, the curing agent is added into the component in the step (8) according to the proportion, and the coating operation is carried out after the curing agent is uniformly stirred.
Example 3
This example prepares a titanium dioxide nanocarbon composite static conductive and heat dissipation coating. The used raw materials comprise the following components in parts by weight:
the preparation process comprises the following steps:
(1) dispersing the carbon nano tube in isopropanol solution, carrying out ultrasonic dispersion for 0.5h, adding divinyl triamine, and stirring uniformly.
(2) Adding isobutyl titanate into the solution obtained in the step (1), stirring uniformly, and adding distilled water for dilution.
(3) And (3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction, controlling the temperature of the hydrothermal reaction to be 200-250 ℃ and the time to be 24-26 h. And (3) growing the titanium dioxide nanosheet on the surface of the carbon nanotube in situ to form a composite conductive film solution similar to a sandwich structure.
(4) And (4) carrying out centrifugal operation on the composite conductive film solution obtained in the step (3), and carrying out vacuum drying at the temperature of 60-80 ℃ to obtain the composite nano filler.
(5) And (4) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion for 0.5-1 h to obtain a premix A.
(6) And adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B.
(7) And (4) putting the premix A obtained in the step (5) and the premix B obtained in the step (6) into a mixer, stirring at a high speed for 1-1.5 h, and physically mixing to obtain a mixed material.
(8) And (4) putting the mixed material obtained in the step (7) into a three-roller machine, grinding for 2-3 h, taking out, sealing and bottling to obtain the titanium dioxide nano-carbon composite static conductive and heat dissipation coating.
(9) When in use, the curing agent is added into the component in the step (8) according to the proportion, and the coating operation is carried out after the curing agent is uniformly stirred.
And (3) carrying out performance test on the coating:
and (4) testing standard: the surface resistivity is determined according to GB/T169906 & 1997 petroleum tank conductive electrostatic coating resistivity determination method; adhesion Standard GB/T9286 1998 test for marking test of paint films of paints and varnishes; oil resistance standard GB/T1734-1993 gasoline resistance determination of paint film; the emissivity is tested using a hemispherical emissivity detector.
Comparative example 1:
no in situ titanium dioxide was introduced in the formulation of example 1, titanium dioxide being absent
Comparative example 2:
in the formulation of example 1, no in-situ titanium dioxide was introduced, and nano-titanium dioxide was used instead of direct mixing
And (3) carrying out performance test on the coating:
the embodiment 1 and the comparative examples 1 and 2 show that the titanium dioxide nano-ions grown in situ on the surface of the carbon nano-tube are beneficial to improving the conductivity of the coating and improving the heat radiation and heat dissipation capacity; meanwhile, the compatibility of the resin and the carbon nanotube material is improved by the in-situ growth method, the binding force is increased, the adhesive force is improved, and the oil resistance is improved.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (13)
1. A preparation method of titanium dioxide nano carbon composite static conductive heat dissipation coating is characterized by comprising the following steps:
(1) dispersing carbon nano tubes in isopropanol solution, adding divinyl triamine and uniformly stirring;
(2) adding titanate into the solution obtained in the step (1), uniformly stirring, and adding distilled water for dilution;
(3) putting the solution obtained in the step (2) into a hydrothermal reaction kettle for hydrothermal reaction to obtain a composite conductive filler solution;
(4) carrying out centrifugal operation on the composite conductive filler solution obtained in the step (3), and drying the solid to obtain a composite nano filler;
(5) mixing the composite nano filler obtained in the step (4), mica powder, fumed silica, a nano dispersant, a flatting agent and a defoaming agent, adding half of xylene, n-butyl alcohol and butyl acetate solvent, and performing ultrasonic dispersion to obtain a premix A;
(6) adding the rest xylene, n-butanol and butyl acetate solvent into the epoxy resin for dilution to obtain a premix B;
(7) physically mixing the premix A and the premix B to obtain a mixed material;
(8) grinding the mixed material obtained in the step (7) in a three-roller machine to obtain the titanium dioxide nano carbon composite static conductive and heat dissipation coating;
(9) when in use, the curing agent is added into the components in the step (8) according to the proportion, and the coating operation can be carried out after the curing agent is uniformly stirred;
wherein the weight parts of the raw materials are as follows:
30-50 parts of epoxy resin; 10-30 parts of a curing agent; 30-50 parts of titanate; 3-10 parts of carbon nanotubes; 5-10 parts of mica powder; 1-3 parts of fumed silica; 1-10 parts of a nano dispersant; 0.1-1 part of a leveling agent; 0.1-0.5 part of defoaming agent; 30-50 parts of dimethylbenzene; 30-50 parts of n-butyl alcohol; 30-50 parts of isopropanol; 3-1.5 parts of divinyl triamine; 10-20 parts of butyl acetate; 80-100 parts of distilled water.
2. The method of claim 1, wherein the epoxy resin is a fluorine-modified epoxy resin E-20 or epoxy resin E-44 or a mixture thereof.
3. The process according to claim 1, wherein the titanate is isobutyl titanate, isopropyl titanate or tetra-n-butyl titanate.
4. The method according to claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes having a diameter of 10 to 100 nm.
5. The method of claim 1, wherein the carbon nanotubes are dispersed in the isopropanol solution by sonication in step (1).
6. The method of claim 5, wherein the sonication time is 0.5 h.
7. The preparation method according to claim 1, wherein the hydrothermal reaction in the step (3) is carried out at a temperature of 200-250 ℃ for 24-26 hours.
8. The method according to claim 1, wherein the drying in the step (4) is vacuum drying at 60 to 80 ℃.
9. The preparation method according to claim 1, wherein the time for the ultrasonic dispersion in the step (5) is 0.5 to 1 hour.
10. The method of claim 1, wherein the physical mixing in step (7) comprises: and (3) putting the premix A and the premix B into a mixer, stirring at a high speed for 1-1.5 h, and physically mixing.
11. The method according to claim 1, wherein the particle size of the paint ground in the step (8) is 3 to 5 μm.
12. The method according to claim 1, wherein the grinding time in step (8) is 2 to 3 hours.
13. The titanium dioxide nano carbon composite static conductive and heat dissipation coating prepared by the preparation method of any one of claims 1 to 12.
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