CN108976877B - Gradient conductive coating and preparation method thereof - Google Patents
Gradient conductive coating and preparation method thereof Download PDFInfo
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- CN108976877B CN108976877B CN201810757574.1A CN201810757574A CN108976877B CN 108976877 B CN108976877 B CN 108976877B CN 201810757574 A CN201810757574 A CN 201810757574A CN 108976877 B CN108976877 B CN 108976877B
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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
- 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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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- 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
- C08K2201/001—Conductive additives
Abstract
The invention discloses a gradient conductive coating, which comprises a high polymer base material, a carbon material and a curing agent, wherein the carbon material is carbon black or carbon nano tubes, and the high polymer base material is epoxy resin, unsaturated resin or polyurethane. The preparation method comprises the following steps: firstly, preparing a carbon material bottom layer, performing sand blasting pretreatment on the surface of a substrate, and then brushing the carbon material bottom layer on the surface of the substrate; and when 10-30% of film-forming substances on the surface of the matrix are cured, sequentially brushing the middle layer and the upper layer of the carbon material on the surface of the matrix, and finally, settling and curing the coating. The method ensures that the conductive particles are uniformly dispersed in the coating, so that the coating does not generate honeycombs or air holes, the coating has high bonding strength, and can conduct electricity under the condition of small content of a conductive medium, thereby improving the anticorrosion effect of the matrix.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a gradient conductive coating and a preparation method thereof.
Background
The surface of petrochemical equipment is coated with a conductive coating, so that the corrosion of the equipment can be prevented, and the ignition caused by spark generated by static electricity can also be prevented, and as the conductive coating has to have an anti-corrosion function, generally, the thicker the coating is, the better the corrosion resistance is, so that the anti-corrosion coating is generally coated for 2-3 times on the metal surface to ensure the thickness of the coating. The conductive coating is different from common organic paint, and mainly uses non-metal high polymer with anticorrosion effect as film-forming material, and uses metal particles or carbon material as conductive medium and fills them in the high polymer, after the high polymer is solidified, the high polymer coating containing conductive particles can be formed, so that the conductive anticorrosion effect can be reached. Most of the conductive metal particles or carbon substances are Cu powder, Ag powder, carbon black, carbon fibers and carbon nanotubes, and because the specific gravity of the metal particles is large, the metal particles are easy to precipitate after being mixed with organic high polymers, particularly in the coating construction process, the metal particles are easy to precipitate at the bottom of the coating due to the action of gravity, the bonding strength of the coating and a substrate is reduced after the metal particles are precipitated at the bottom, and the coating is easy to peel and fall off; in addition, the conductive metal particles are deposited on the bottom of the coating, and the surface of the coating contains no or few conductive particles, so that the conductivity of the coating can hardly meet the standard requirement. The carbon fiber is used as a conductive medium, and is easy to expose outside the coating to form burrs, so that the surface of the coating is not smooth. In view of the above practical problems, most petrochemical anticorrosive conductive coatings use carbon black or carbon nanotubes as the conductive medium, the carbon black or carbon nanotubes have small diameter and light specific gravity, and can meet the conductive requirement by adding a small amount of the carbon black or carbon nanotubes in the coating. However, since carbon black or carbon nanotubes have small particle size and high surface energy and are easily agglomerated, the mass of the agglomerated carbon black or carbon nanotubes is increased, and precipitates are generated during coating construction, so that conductive particles at the bottom of a coating are increased after the precipitates are precipitated, conductive particles on the surface are reduced, and the conductive requirements cannot be met, in order to solve the problems, more carbon black or carbon nanotube conductive particles are required to be added, and when the conductive carbon black or carbon nanotubes are excessively added, the viscosity of an organic high polymer is increased on one hand, and the construction is inconvenient; on the other hand, the increase of the agglomerates enables the coating to generate honeycombs or air holes, the anticorrosion effect of the coating is influenced, and particularly for a thicker anticorrosion coating, the honeycombs generated at the bottom of the coating are more obvious, so that the coating is brittle and the adhesive force is greatly reduced.
Disclosure of Invention
The invention aims to provide a gradient conductive coating, which solves the problems of uneven dispersion and low adhesion of conductive particles in the conventional conductive coating.
The invention also aims to provide a preparation method of the gradient conductive coating.
The technical scheme adopted by the invention is that the gradient conductive coating comprises a high polymer base material, a carbon material and a curing agent; the carbon material is carbon black or carbon nano-tube; the high polymer base material is epoxy resin, unsaturated resin or polyurethane.
The invention adopts another technical scheme that a preparation method of the gradient conductive coating is implemented according to the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.005-0.006 parts of high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material bottom layer;
step 2, carrying out sand blasting pretreatment on the surface of the matrix;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.008-0.009 high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material middle layer;
step 5, when 10-30% of the film forming material on the surface of the substrate in the step 3 is solidified, brushing the carbon material middle layer obtained in the step 4 on the surface of the substrate in the step 3;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.1-0.15: 0.009 mixing the high polymer base material, the diluent and the carbon material uniformly, then adding the curing agent, and stirring for 3-5 min to obtain an upper layer of the carbon material;
7, when 10% -30% of the film-forming substances on the surface of the substrate in the step 4 are cured, coating the upper layer of the carbon material obtained in the step 6 on the surface of the substrate in the step 5;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
The present invention is also characterized in that,
in the steps 1, 4 and 6, carbon materials are carbon black or carbon nano tubes; the high polymer base material is epoxy resin, unsaturated resin or polyurethane.
In the steps 1, 4 and 6, mechanical stirring is adopted during mixing, and the stirring time is 1-2 h; or all the ultrasonic vibration is adopted, and the vibration time is 1-2 h.
In the step 2, the concrete steps are as follows: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.4-0.7 MPa, the grinding material is 16-18 meshes of carborundum, and then blowing off floating ash on the surface of the matrix by adopting high-pressure air.
In the step 3, the step 5 and the step 7, the thickness of the coating is controlled to be 0.1 mm-0.3 mm.
The method has the advantages that the method ensures that the conductive particles are uniformly dispersed in the coating, so that the coating does not generate honeycombs or air holes, the coating has high bonding strength, and can conduct electricity under the condition of small content of a conductive medium, thereby improving the anticorrosion effect of the matrix.
Drawings
FIG. 1 is a TEM image of a single-layer carbon nanotube prepared by the method of the present invention;
FIG. 2 is a TEM image of a two-layered carbon nanotube prepared by the method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a gradient conductive coating, which comprises a high polymer base material, a carbon material and a curing agent;
the carbon material is carbon black or carbon nano-tube;
the high polymer base material is epoxy resin, unsaturated resin or polyurethane.
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.005-0.006 parts of high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material bottom layer;
the carbon material is carbon black or carbon nano-tube;
the high polymer base material is epoxy resin, unsaturated resin or polyurethane;
during mixing, mechanical stirring is adopted, and the stirring time is 1-2 h; or ultrasonic vibration is adopted, and the vibration time is 1-2 h;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.4-0.7 MPa, the grinding material is 16-18 meshes of carborundum, and then blowing off floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.1-0.3 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.008-0.009 high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material middle layer;
the carbon material is carbon black or carbon nano-tube;
the high polymer base material is epoxy resin, unsaturated resin or polyurethane;
during mixing, mechanical stirring is adopted, and the stirring time is 1-2 h; or ultrasonic vibration is adopted, and the vibration time is 1-2 h;
step 5, when 10-30% of the film forming material on the surface of the substrate in the step 3 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the carbon material middle layer obtained in the step 4 is coated on the surface of the substrate in the step 3, and the thickness of the coating is controlled to be 0.1-0.3 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.1-0.15: 0.009 mixing the high polymer base material, the diluent and the carbon material uniformly, then adding the curing agent, and stirring for 3-5 min to obtain an upper layer of the carbon material;
during mixing, mechanical stirring is adopted, and the stirring time is 1-2 h; or ultrasonic vibration is adopted, and the vibration time is 1-2 h;
7, when 10-30% of the film forming material on the surface of the substrate in the step 4 is cured, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.1-0.3 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
The curing agent adopted by the high polymer base material is a curing agent corresponding to conventional epoxy resin, unsaturated resin or polyurethane, and the dosage ratio of the curing agent is irrelevant to the content of the conductive carbon material.
A TEM image of a single-layer carbon nanotube prepared by the method of the present invention is shown in fig. 1, where the content of the carbon nanotube in the image is 0.5 wt.%, as shown in fig. 1, when there is only one layer, the top carbon nanotube is less, the bottom carbon nanotube is more, the carbon nanotube is unevenly distributed in the coating layer, the bottom carbon nanotube makes the bonding strength of the coating poor, and the top carbon nanotube is less, so the coating is poor in conductivity, and therefore 0.5 wt.% of carbon black or carbon nanotube cannot successfully prepare the conductive coating, if the content of the conductive particle is increased, the content of the conductive particle at the bottom is inevitably higher, the bonding strength of the coating is worse, and the coating is thicker, the conductive particle layer is more serious, so that the conductive coating cannot be prepared by using a one-time brushing method.
According to a TEM image of the two-layer carbon nanotube prepared by the method, as shown in FIG. 2, the content of the conductive particles of the carbon nanotube at the bottom layer is 0.5 wt.%, and the content of the conductive particles of the carbon nanotube at the upper layer is 0.8 wt.%, so that the content of the conductive particles at the upper layer is more than 0.5 wt.% due to the fact that the conductive particles at the upper layer penetrate through an interface between the two layers, and the conductive particles penetrate through the upper layer from the top of the bottom layer, so that the non-conductive bottom layer is conductive, and the uniform distribution of the conductive particles is achieved. By multiple brushing, the thicker conductive coating can be prepared, and the conductivity and the bonding strength can meet the requirements of the conductive coating.
TABLE 1 bonding Strength of conductive composite coatings with different conductive Filler contents to Metal substrates
As can be seen from table 1, the bond strength of the coating decreases with increasing conductive carbon media, but the bond strength after the gradient coating (i.e., the present method) used is comparable to a single layer; as can be seen from table 2, the resistance is greatest when the conductive carbon particle content in the monolayer is 0.6 wt.%, and the resistance of the coating is least when the conductive carbon particle content is 0.9 wt.%, but with the conductive carbon particle content of the bottom layer being 0.6 wt.%, and the conductive carbon particle content of the intermediate layer and the top layer being 0.9 wt.%, the resistance is less than the conductive carbon particle content of the layers by 0.9 wt.% and greater than the conductive carbon particle content of the intermediate layer by 0.6 wt.%, indicating that the conductive particles of the top layer and the intermediate layer cross the interlayer interface.
TABLE 2 thickness and resistivity of conductive composite coatings with different conductive filler content
According to the invention, by adding a method of adding less conductive particles and more surface conductive particles to the bottom layer, aggregation and sinking of the conductive particles in the coating curing process are well prevented, so that the problems of less surface conductive particles and more bottom conductive particles are solved, the problems of honeycombing of the coating and low coating bonding strength caused by more bottom conductive particles are solved, and the problems of less surface conductive particles and high resistivity of the coating, namely non-conductivity, are also solved.
The method of the invention coats the middle layer or the surface layer before the paint is not solidified, which solves the problem that the conductive particles sink in the paint solidification process, the conductive particles of the bottom layer are increased from 0.5 wt.% to 0.7-0.8 wt.% contained in the original paint, the conductive particles of the bottom layer surface can not reach 0.5-0.6 wt.%, if the concentration of the conductive particles in the paint is lower than 0.5-0.6 wt.%, the coating can not conduct electricity, and thus the conductivity and the bonding strength of the conductive paint can not meet the use requirements. When the primer is in a semi-dry state, the conductive particles on the upper layer are deposited and can penetrate through the interface between the two layers, so that the concentration of the conductive particles on the surface of the lower layer coating reaches 0.6 wt.%, the conductive particles on the upper layer are high in content, the conductive particles on the upper layer sink to the lower layer, and the conductive particles on the upper layer can also contain more than 0.6 wt.%, so that the conductive particles are basically and uniformly distributed in the whole coating to be about 0.6 wt.%.
Example 1
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.1: uniformly mixing 0.005 of epoxy resin E44, acetone and carbon black, adding a diethylenetriamine curing agent, and stirring for 3min to obtain a carbon material bottom layer;
during mixing, mechanical stirring is adopted, and the stirring time is 1 h;
the mass ratio of the diethylenetriamine curing agent to the epoxy resin E44 is 1: 0.1;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.4MPa, the grinding material is 16-mesh carborundum, and then blowing off floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.1 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.1: uniformly mixing 0.008 epoxy resin E44, acetone and carbon black, adding a diethylenetriamine curing agent, and stirring for 3min to obtain a carbon material middle layer;
during mixing, mechanical stirring is adopted, and the stirring time is 1 h;
the mass ratio of the diethylenetriamine curing agent to the epoxy resin E44 is 1: 0.1;
step 5, when 10% of the film forming material on the surface of the substrate in the step 3 is solidified, namely the diluent is completely volatilized, the carbon material obtained in the step 4 is coated on the surface of the substrate in the step 3 in a middle layer mode, and the thickness of the coating is controlled to be 0.1 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.1: uniformly mixing 0.009 epoxy resin E44, acetone and carbon black, adding diethylenetriamine curing agent, and stirring for 3min to obtain an upper layer of carbon material;
the mass ratio of the diethylenetriamine curing agent to the epoxy resin E44 is 1: 0.1;
during mixing, mechanical stirring is adopted, and the stirring time is 1 h;
7, when 10% of the film forming material on the surface of the substrate in the step 4 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the upper layer of the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.1 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
Example 2
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.12: 0.005 of 196 unsaturated resin, styrene and carbon nano tubes are uniformly mixed, and then methyl ethyl ketone peroxide curing agent is added and stirred for 3min to obtain a carbon material bottom layer;
the mass ratio of the methyl ethyl ketone peroxide curing agent to the 196 unsaturated resin is 1: 0.02;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1 h;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.5MPa, the grinding material is 16-mesh carborundum, and then blowing floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.1 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.13: 0.009 of 196 unsaturated resin, styrene and carbon nano tubes are uniformly mixed, and then methyl ethyl ketone peroxide curing agent is added and stirred for 4min to obtain a carbon material middle layer;
the mass ratio of the methyl ethyl ketone peroxide curing agent to the 196 unsaturated resin is 1: 0.02;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1.5 h;
step 5, when 20% of the film forming material on the surface of the substrate in the step 3 is solidified, namely the diluent is completely volatilized, the carbon material obtained in the step 4 is coated on the surface of the substrate in the step 3 in a middle layer mode, and the thickness of the coating is controlled to be 0.2 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.12: 0.009 of 196 unsaturated resin, styrene and carbon nano tube are uniformly mixed, and then methyl ethyl ketone peroxide curing agent is added and stirred for 3min to obtain an upper layer of carbon material;
the mass ratio of the methyl ethyl ketone peroxide curing agent to the 196 unsaturated resin is 1: 0.02;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1.5 h;
7, when 20% of the film forming material on the surface of the substrate in the step 4 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the upper layer of the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.2 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
Example 3
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.14: uniformly mixing 196 unsaturated resin of 0.006, styrene and carbon nano tubes, adding a cobalt naphthenate peroxide curing agent, and stirring for 4min to obtain a carbon material bottom layer;
the mass ratio of cobalt naphthenate-containing methyl ethyl ketone peroxide curing agent to 196 unsaturated resin is 1: 0.0002;
during mixing, mechanical stirring is adopted, and the stirring time is 1.5 h;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.6MPa, the grinding material is 18-mesh carborundum, and then blowing floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.2 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.14: uniformly mixing 196 parts of unsaturated resin of 0.008, styrene and carbon nano tubes, adding a cobalt naphthenate peroxide methyl ethyl ketone curing agent, and stirring for 5min to obtain a carbon material middle layer;
the mass ratio of cobalt naphthenate-containing methyl ethyl ketone peroxide curing agent to 196 unsaturated resin is 1: 0.0002;
during mixing, mechanical stirring is adopted, and the stirring time is 1.5 h;
step 5, when 15% of the film forming material on the surface of the substrate in the step 3 is solidified, namely the diluent is completely volatilized, the carbon material obtained in the step 4 is coated on the surface of the substrate in the step 3 in a middle layer mode, and the thickness of the coating is controlled to be 0.2 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.12: 0.009 of 196 unsaturated resin, styrene and carbon nano tube are uniformly mixed, and then methyl ethyl ketone peroxide curing agent containing cobalt naphthenate is added and stirred for 5min to obtain an upper layer of the carbon material;
the mass ratio of cobalt naphthenate-containing methyl ethyl ketone peroxide curing agent to 196 unsaturated resin is 1: 0.0002;
during mixing, mechanical stirring is adopted, and the stirring time is 1.5 h;
7, when 30% of the film forming material on the surface of the substrate in the step 4 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the upper layer of the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.3 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
Example 4
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.14: uniformly mixing 0.006 parts of epoxy resin E44, acetone and carbon nano tubes, adding a diamine curing agent, and stirring for 5min to obtain a carbon material bottom layer;
the mass ratio of the hexamethylene diamine curing agent to the epoxy resin E44 is 1: 0.07;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1.5 h;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.6MPa, the grinding material is 16-mesh carborundum, and then blowing floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.1 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.14: uniformly mixing 0.008 epoxy resin E44, acetone and carbon nanotubes, adding a diamine curing agent, and stirring for 5min to obtain a carbon material middle layer;
the mass ratio of the hexamethylene diamine curing agent to the epoxy resin E44 is 1: 0.07;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1.5 h;
step 5, when 30% of the film forming substances on the surface of the substrate in the step 3 are solidified, namely the diluent is completely volatilized, the carbon material obtained in the step 4 is coated on the surface of the substrate in the step 3 in a middle layer mode, and the thickness of the coating is controlled to be 0.1 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.14: 0.009 epoxy resin E44, acetone and carbon nano tube are uniformly mixed, and then diamine curing agent is added and stirred for 3min to obtain an upper layer of carbon material;
the mass ratio of the hexamethylene diamine curing agent to the epoxy resin E44 is 1: 0.07;
during mixing, ultrasonic vibration is adopted, and the vibration time is 1.5 h;
7, when 30% of the film forming material on the surface of the substrate in the step 4 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the upper layer of the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.1 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
Example 5
The invention relates to a preparation method of a gradient conductive coating, which is implemented by the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.15: uniformly mixing 0.006% polyurethane, ethyl acetate and carbon nanotubes, adding a matched curing agent, and stirring for 5min to obtain a carbon material bottom layer;
the mass ratio of the curing agent to the polyurethane is 1: 0.5;
during mixing, mechanical stirring is adopted, and the stirring time is 2 hours;
the polyurethane manufacturer is Jining HuaKai resin Co., Ltd;
step 2, carrying out sand blasting pretreatment on the surface of the matrix: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.7MPa, the grinding material is 18-mesh carborundum, and then blowing floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2, and controlling the thickness of the coating to be 0.3 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.15: 0.009 polyurethane, ethyl acetate and carbon nano tube are uniformly mixed, and then a curing agent is added and stirred for 5min to obtain a carbon material middle layer;
the mass ratio of the curing agent to the polyurethane is 1: 0.5;
during mixing, mechanical stirring is adopted, and the stirring time is 2 hours;
step 5, when 30% of the film forming substances on the surface of the substrate in the step 3 are solidified, namely the diluent is completely volatilized, the carbon material obtained in the step 4 is coated on the surface of the substrate in the step 3 in a middle layer mode, and the thickness of the coating is controlled to be 0.3 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.15: 0.009 polyurethane, ethyl acetate and carbon nano tube are uniformly mixed, and then a curing agent is added and stirred for 3min to obtain an upper layer of carbon material;
the mass ratio of the curing agent to the polyurethane is 1: 0.5;
during mixing, mechanical stirring is adopted, and the stirring time is 2 hours;
7, when 30% of the film forming material on the surface of the substrate in the step 4 is solidified, namely the diluent is completely volatilized, the surface is in a semi-dry state, the surface coating does not flow, when a finger presses the substrate to slightly stick the finger, the upper layer of the carbon material obtained in the step 6 is coated on the surface of the substrate in the step 5, and the thickness of the coating is controlled to be 0.3 mm;
and 8, settling and curing: and (3) curing the coating obtained in the step (7) at room temperature for 3 hours to obtain the gradient conductive coating.
The method ensures that the conductive particles are uniformly dispersed in the coating, so that the coating does not generate honeycombs or air holes, the coating has high bonding strength, and can conduct electricity under the condition of small content of a conductive medium, thereby improving the anticorrosion effect of the matrix.
Claims (2)
1. The preparation method of the gradient conductive coating is characterized by comprising the following steps:
step 1, preparing a carbon material bottom layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.005-0.006 parts of high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material bottom layer;
step 2, carrying out sand blasting pretreatment on the surface of the matrix; the method comprises the following specific steps: carrying out sand blasting and coarsening treatment on the surface of the matrix, wherein the sand blasting pressure is 0.4-0.7 MPa, the grinding material is 16-18 meshes of carborundum, and then blowing off floating ash on the surface of the matrix by adopting high-pressure air;
step 3, brushing the carbon material bottom layer obtained in the step 1 on the surface of the substrate pretreated in the step 2; the thickness of the coating is controlled to be 0.1 mm-0.3 mm;
step 4, preparing a carbon material middle layer: mixing the components in a mass ratio of 1: 0.1-0.15: uniformly mixing 0.008-0.009 high polymer base material, diluent and carbon material, then adding curing agent, and stirring for 3-5 min to obtain a carbon material middle layer;
step 5, when 10-30% of the film forming material on the surface of the substrate in the step 3 is solidified, brushing the carbon material middle layer obtained in the step 4 on the surface of the substrate in the step 3; the thickness of the coating is controlled to be 0.1 mm-0.3 mm;
step 6, preparing an upper layer of the carbon material: mixing the components in a mass ratio of 1: 0.1-0.15: 0.009 mixing the high polymer base material, the diluent and the carbon material uniformly, then adding the curing agent, and stirring for 3-5 min to obtain an upper layer of the carbon material;
7, when 10% -30% of the film-forming substances on the surface of the substrate in the step 4 are cured, coating the upper layer of the carbon material obtained in the step 6 on the surface of the substrate in the step 5; the thickness of the coating is controlled to be 0.1 mm-0.3 mm;
and 8, settling and curing: curing the coating obtained in the step 7 at room temperature for 3 hours to obtain a gradient conductive coating;
in the steps 1, 4 and 6, carbon materials are carbon black or carbon nano tubes; the high polymer base material is epoxy resin, unsaturated resin or polyurethane.
2. The method for preparing a gradient conductive coating according to claim 1, wherein in the steps 1, 4 and 6, mechanical stirring is adopted during mixing, and the stirring time is 1-2 h; or all the ultrasonic vibration is adopted, and the vibration time is 1-2 h.
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