CN104449239A - Nitrogen-doped graphene composited electromagnetic shielding type electricity conductive primer and preparation method thereof - Google Patents

Nitrogen-doped graphene composited electromagnetic shielding type electricity conductive primer and preparation method thereof Download PDF

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Publication number
CN104449239A
CN104449239A CN201410796032.7A CN201410796032A CN104449239A CN 104449239 A CN104449239 A CN 104449239A CN 201410796032 A CN201410796032 A CN 201410796032A CN 104449239 A CN104449239 A CN 104449239A
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preparation
electromagnetic shielding
epoxy resin
component
priming paint
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薛卫东
赵睿
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SICHUAN HUANTAN TECHNOLOGY Co Ltd
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SICHUAN HUANTAN TECHNOLOGY Co Ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24Electrically-conducting paints
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/20Diluents or solvents
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    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/47Levelling agents
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

Abstract

The invention discloses a preparation method of electromagnetic shielding type electricity conductive primer. The method comprises the steps of a, diluting epoxy resin through a diluent, and feeding the epoxy resin and the diluent to a high-speed agitating diffuser to heat and agitate until dissolving; b, feeding a diluent of which the volume is 3 to 3.5 times that of the epoxy resin after the dissolution is completely done, continuously agitating, respectively feeding conductive packing, a nitrogen-doped graphene/ nano-metal composite material after the obtained liquid is uniformly agitated, and then feeding a coating additive while agitating at a high speed; c, continuously agitating at a high speed, then feeding activated organobentonite of which the mass is 0.2 to 1.5% of that of the liquid, and feeding 0.02 to 0.5% of flatting agent at the same time, agitating at a high speed, and then feeding the obtained liquid into a container to be used as a component A for later use; d, preparing a T31 epoxy resin curing agent as a component B, quickly uniformly mixing, and then spraying, wherein the volume of the component B is 3% of that of the component A during use. With the adoption of the preparation method, the glossiness and the ageing resistance of the conductive primer can be raised; the weather resistance and the corrosion resistance of a coating are improved; and outstanding conductivity and temperature and humidity resistance are obtained.

Description

Electromagnetic shielding conductive priming paint of a kind of azepine Graphene compound and preparation method thereof
Technical field
The invention belongs to electromagnetic-shielding conductive coating field, be specifically related to electromagnetic shielding conductive priming paint of azepine Graphene compound and preparation method thereof.
Background technology
In recent years, the housing of electronic product (as robot calculator, communication equipment, office equipment, household electrical appliance and medical facilities etc.) and aviation aircraft adopt more and more light weight, easily machine-shaping macromolecular material manufacture to replace traditional metallic substance, but macromolecular material is generally isolator, itself shielding effect is had no to electromagnetic interference, the micro-current power of electronics is close with electromagnetic noise power, very easily by outside electromagnetic interference.Be that the Electromagnetic Interference of the various electronic products of housing is also on the rise with macromolecular material, electromagnetic interference is affecting the life of people.The World Health Organization (WHO) is classified as electromagnetic radiation pollution as the fourth-largest pollution after water, gas, sound.
Along with the develop rapidly of electronic industry, the electromagnetic interference (EMI) caused by hertzian wave and electromagnetic compatibility (EMC) not only have a strong impact on electrically and the normal operation of electronics, also the serious threat health of the mankind.In order to solve the problem of plastic casing electromagnetism interference, generally adopt the method for metallization of plastic surface.Wherein electrically conducting coating can spray or brush the plastic part surface in different shape easily, forms the coating for EMI shielding of conduction, becomes electromagnetic shielding material most widely used at present.Electrically conducting coating is formulated by synthetic resins, conductive filler material, solvent.Be coated on substrate surface and formed one deck cured film, thus produced conductive effect.According to composition and the difference of electrical conduction mechanism, electrically conducting coating can be divided into structure-type and mixed type two kinds.Wherein mixed type electrically conducting coating is the main Types of application at present, and its conductivity principle mainly contains two: (1) conductive channel principle.Namely the realization of conductive coating conducting function is by contacting with each other between conductive filler particles, is overlapped to form chain and latticed 3 D stereo conductive structure, forms the conductive channel that can transmit electronics.After the conductive filler particles concentration of adding in electrically conducting coating reaches seepage flow threshold value, contact with each other between a large amount of conductive filler particles, make electronics displacement under the carrying of current carrier form electric current, realize the conductivity of final coating.As patent CN101515486A, CN101108947A, CN101824241A etc.The shortcoming of this kind of electrically conducting coating is that conductive filler particles concentration is large, and namely conductive filler material amount requires large, could form electric current after need reaching seepage flow threshold value.Therefore, coating is heavier, thicker.(2) tunnel effect principle.Namely the gap in coating between conductive filler particles fill by the high molecular polymer of insulativity, when the thickness of megohmite is thinned to about 10 ran, electronics just under the effect of electric field displacement form electric current, thus make coated conductive.Tunnel effect theory is thought, the realization of Electrical Conductivity of Conductive Coating energy comes from the displacement of electronics under internal electric field or thermal vibration effect to form electric current.As patent CN1796477A, CN101210124A, CN102850885A etc.And the shortcoming of this kind of electrically conducting coating is the electric current that electronics is formed under electric field or thermal vibration effect by tunnel effect, the conductivity of this material is comparatively front a kind of poor, is generally used in antistatic coating.
Graphene be monolayer carbon atom tightly packed and formed a kind of carbonaceous novel material.Chemically on bonding pattern, form the carbon atom of Graphene two-dirnentional structure with sp 2mode hydridization, this hybrid form makes carbon atom and adjacent three carbon atoms form stable C ~ C key by σ key, imparts the mechanical property that Graphene is high.Form large π key in the π-electron delocalization provided perpendicular to carbon atom a large amount of on graphene planes, electronics can move freely wherein simultaneously, and therefore Graphene all has excellent electroconductibility usually, and its carrier mobility speed is up to 2 × 10 5cm 2v -1s -1deng.Graphene is thin, the hardest nano material in known world, it is almost completely transparent, there is the advantages such as thermal conductivity is high, resistivity is low, flexility is good, be therefore used as the conduction adding material (as CN102977742A etc.) of coating in recent years.
The present invention is directed to current electromagnetic shielding conductive coating lay particular stress on, partially thick, unstable and the problem such as on the weak side of conductivity, adopt the azepine graphene/nanometer metal composite (see Chinese patent CN103663441A) prepared by solid phase cleavage method by metal phthalocyanine complex as conduction adding material and flexibility agent, prepare the electromagnetic shielding conductive material that a kind of top coat is frivolous, weathering resistance is strong.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency existing in prior art, the technical problem providing a kind of the present invention to solve is electromagnetic shielding conductive priming paint providing a kind of good conductivity, strong adhesion, good weatherability, coating frivolous and preparation method thereof.
In view of this, the invention provides a kind of electromagnetic shielding conductive priming paint preparation method of azepine Graphene compound, comprise the following steps:
A, use thinner dilution epoxy resin, the decollator heated and stirred the two added with high-speed stirring is dissolved;
After b, dissolving completely, then the thinner adding epoxy resin volume 3 ~ 3.5 times continues to stir, and adds conductive filler material, azepine graphene/nanometer metal composite respectively, add coatings additive(s) under high velocity agitation after gained solution stirring is even;
C, continue the organobentonite adding activated process after high-speed stirring, add that quality is solution quality 0.2 ~ 1.5%, and the flow agent of 0.02 ~ 0.5%, after high-speed stirring, the solution obtained is put into container stand-by as component A;
D, get T31 epoxy curing agent as B component;
B component is measured by 3% of component A volume, for spraying application after short mix is even during use.
Preferably, epoxy resin is E ~ 20 epoxy resin, and content of epoxy resin is 0.8 to 1 times of diluent volume.
Preferably, the thinner in step a by dimethylbenzene and propyl carbinol by volume 5:4 be hybridly prepared into.
Preferably, the conductive filler material in step b is flake silver powder or silver-coated copper powder, and particle diameter is 200 order ~ 250 orders, and its consumption is 10 ~ 30% of solution quality.
Preferably, the azepine graphene/nanometer metal composite in step b is the one in azepine graphene/nano silver matrix material, azepine graphene/nanometer copper composite material, azepine graphene/nanometer nickel composite material, its consumption be solution quality ~ 2%.
Preferably, wherein said coatings additive(s) is titanate coupling agent, and its consumption is 0.2 ~ 1.5% of liquor capacity.
Preferably, the organobentonite of wherein activated process is that particle diameter is below 200 orders, and its consumption is 0.2 ~ 1.5% of solution quality through methyl alcohol sealing active process.
Preferably, wherein flow agent is the one in organic silicon modified by polyether, polyester resin change properties of organic silicon, and its consumption is solution quality 0.02 ~ 0.5%.
Present invention also offers a kind of electromagnetic shielding conductive priming paint of azepine Graphene compound, priming paint prepared by the preparation method of its aforementioned electromagnetic shielding conductive priming paint.
The electric conductivity of aforementioned priming paint is less than 0.4 ohm/sheet resistance.
Wherein azepine graphene/nanometer process for preparing metal composite material carries out with reference to Chinese patent CN103663441A, comprises the following steps:
Step one: with phthalocyanine compound, phthalocyanine polymer and derivative thereof for starting raw material, does not do other Feedstock treating and directly uses.
Step 2: in atmosphere furnace, with under certain gas shield, with reference to the thermochemistry characteristic of raw material, adopt temperature programming method, in catalyst-free condition, once property cracking obtains azepine Graphene class and metallic graphite carbon alkene class material.
Or adopt following method, comprising:
Step one: with phthalocyanine compound, phthalocyanine polymer and derivative thereof for starting raw material, does not do other Feedstock treating and directly uses.
Step 2: in atmosphere furnace, with under certain gas shield, with reference to the thermochemistry characteristic of raw material, adopts temperature programming method, obtains having azepine Graphene class and the metallic graphite carbon alkene class material of coiled structure there being on metal catalysis conditions once property cracking.
Described starting raw material can be commercially available or make metallo phthalocyanine and derivative thereof by oneself.One of preferred magnesium-yttrium-transition metal phthalocyanine-like compound and derivative thereof (as silver-colored in Nickel Phthalocyanine, CuPc, FePC, phthalocyanine molybdenum, Cobalt Phthalocyanine, phthalocyanine gold, phthalocyanine and derivative etc.).
Described starting raw material can also be one of nonmetal phthalocyanine class materials such as pure phthalocyanine compound.
Described starting raw material can also be one of containing metal oxide phthalocyanines material.
Described starting raw material can also be one of polymer or the porphyrin polymkeric substance containing class phthalocyanine ring structure containing phthalocyanine ring structure.
Described gas shield refers at the conventional shielding gas such as nitrogen, argon gas, argon gas/hydrogen mixed gas, argon gas/ammonia gas mixture, nitrogen/hydrogen mixed gas, Nitrogen, Ammonia gas mixture; The concrete ratio of gas mixture is between volume ratio 0.1:9.9 ~ 1:9; Flow rate control is between 10 ~ 50cm3min ~ 1;
Described metal catalyst refers to the metal or alloy such as Copper Foil, copper mesh, nickel foil, nickel foam.
The cracking temperature of described cracking is different according to the thermochemistry characteristic of raw material, is generally more than 700 degree, is preferably 800 ~ 1000 degree.
Under preferred cracking temperature, the time that cracking autocatalysis generates graphene sheet layer is 4 ~ 24 hours, and shorten or extend pyrolysis time to final grapheme material size, thickness and quality have impact.
In azepine Graphene class material, the acquisition of nitrogen element is from self nitrogen-atoms in phthalocyanine frame, obtaining the nitrogen-atoms of more high-content, can pass into the gas mixture of ammonia and rare gas element in cracking process as needed.
In the Graphene class material of containing metal nanoparticle, the acquisition of metal nanoparticle is from metal classification contained by starting raw material self, for CuPc, obtains the grapheme material containing metallic copper nano particle the most at last.
Compared with prior art, the present invention has following features: (1) azepine graphene/nanometer metal composite because of graphene edge azepine and with nano metal compound, inherently there is good conductivity, can add as conductive agent; (2) utilize the active group on azepine graphene sheet layer, with the epoxide group bridging in epoxy resin, the bonding force of coating can be improved on the one hand; Another aspect Graphene not only has sheet structure and size is larger, for micron order, contact the contact that instead of conductive filler material point and point in the past with face with face between electrical conductor, in addition on graphene sheet layer, nano level metal particle is compounded with, and be aided with flake silver powder or silver-coated copper powder, define effective conductive channel of electronics, make conductive primer have good electroconductibility, also can save the consumption of metal powder filler simultaneously; (3) add a small amount of flow agent, not only can improve the levelling property of powder coating, and gloss and the ageing resistance of film can be improved; (4) adopt the E20 epoxy resin of two component, well can be attached to insulating polymeric material (as glass reinforced plastic, polyester chips etc.) surface, and there is good temperature tolerance and wet fastness; (5) add a certain amount of Graphene in the epoxy, not only can improve the snappiness of coating, weathering resistance and the corrosion resistance of coating can be improved simultaneously.
Accompanying drawing illustrates:
The transmission electron microscope picture of Fig. 1 azepine graphene/nanometer copper composite material;
The X-ray diffractogram of Fig. 2 azepine graphene/nanometer copper composite material.
Embodiment
Below in conjunction with test example and embodiment, the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on content of the present invention all belong to scope of the present invention.
In order to understand the present invention further, below in conjunction with specific embodiment, the present invention is described in further detail.When not departing from the above-mentioned thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all within the scope of the present invention.
Production Example 1:
With 30.0 grams of commercially available CuPcs for starting raw material, do not do any purification process.In quartz tube furnace, with under high-purity argon gas protection, argon gas stream speed control is built in 50cm3min ~ 1, and under following intensification scheme, cracking obtains 20.7 grams of final metallic graphite carbon alkene class materials.Namely be warming up to 300 degree with slow heat-up rate 5 degree of per minutes, stablize 1 hour for 300 degree; Be warming up to 350 degree with 5 degree of per minutes, stablize 1 hour for 350 degree; Be warming up to 400 degree with 5 degree of per minutes, stablize 1 hour for 400 degree; Be warming up to 500 degree with 3 degree of per minutes, stablize 4 hours for 500 degree; Be warming up to 800 degree with 2 degree of per minutes, stablize 8 hours for 800 degree, be finally naturally down to room temperature, obtain the Graphene containing metallic copper nano particle.
Production Example 2:
According to the method for Production Example 1, phthalocyanine silver is used to replace the CuPc preparation in Production Example 1 to contain the Graphene of argent nanoparticle.
Embodiment 1
Dimethylbenzene and propyl carbinol by volume 5:4 are hybridly prepared into thinner, measure thinner 491ml, then measure E20 epoxy resin 409ml, and the decollator heated and stirred the two added with high-speed stirring is dissolved, Heating temperature 60 DEG C.Dissolve the thinner adding 1400ml completely to continue to stir, impel whole solution system viscosity to diminish, be easy to fillers dispersed; Add the conductive filler material flaky silver coated copper powder 400 grams after sieving after stirring, azepine graphene/nanometer copper composite material 5 grams, after high-speed stirring 5min, add metatitanic acid coupling agent (HY105) 15ml; Continue the organobentonite 15 grams added after high-speed stirring 5min through activation treatment, organic silicon modified by polyether 3 grams, after high-speed stirring 30min, to put into container stand-by as component A for coating.
B component is T31 epoxy curing agent, measures during use by 3% of component A volume, add component A short mix evenly after namely can be used for spraying application.Its spray-finishing construction method is: on clean vibrin plate substrate, A, B component are mixed fast, reconciling viscosity is about 23 seconds (being coated with ~ 4 glasss), with K ~ 3 spray gun spraying, conductive primer thickness 20 microns, after Air drying solidifies 12 hours, measure the performances such as the electric conductivity (four probe method) of its coating, weathering resistance, sticking power and coating surface appearance, concrete test-results is in table 1.
Embodiment 2
Dimethylbenzene and propyl carbinol by volume 5:4 are hybridly prepared into thinner, measure thinner 491ml, then measure E20 epoxy resin 409ml, and the decollator heated and stirred the two added with high-speed stirring is dissolved, Heating temperature 70 DEG C.Dissolve the thinner adding 1400ml completely to continue to stir, impel whole solution system viscosity to diminish, be easy to fillers dispersed; Add the conductive filler material flake silver powder 350 grams after sieving after stirring, 3 grams, azepine graphene/nano silver matrix material, after high-speed stirring 5min, add metatitanic acid coupling agent (HY105) 15ml; Continue the organobentonite 15 grams added after high-speed stirring 5min through activation treatment, organic silicon modified by polyether 4 grams, after high-speed stirring 30min, to put into container stand-by as component A for coating.
B component is T31 epoxy curing agent, measures during use by 3% of component A volume, add component A short mix evenly after namely can be used for spraying application.Concrete spray-finishing construction method and method for testing performance are with embodiment 1, and its test-results is in table 1.
Embodiment 3
Dimethylbenzene and propyl carbinol by volume 5:4 are hybridly prepared into thinner, measure thinner 491ml, then measure E20 epoxy resin 409ml, and the decollator heated and stirred the two added with high-speed stirring is dissolved, Heating temperature 65 DEG C.Dissolve the thinner adding 1400ml completely to continue to stir, impel whole solution system viscosity to diminish, be easy to fillers dispersed; Add the conductive filler material flake silver powder 420 grams after sieving after stirring, 4 grams, azepine graphene/nano silver matrix material, after high-speed stirring 5min, add metatitanic acid coupling agent (HY105) 15ml; Continue the organobentonite 15 grams added after high-speed stirring 5min through activation treatment, polyester resin change properties of organic silicon 3 grams, after high-speed stirring 30min, to put into container stand-by as component A for coating.
B component is T31 epoxy curing agent, measures during use by 3% of component A volume, add component A short mix evenly after namely can be used for spraying application.Concrete spray-finishing construction method and method for testing performance are with embodiment 1, and its test-results is in table 1.
Embodiment 4
Dimethylbenzene and propyl carbinol by volume 5:4 are hybridly prepared into thinner, measure thinner 491ml, then measure E20 epoxy resin 409ml, and the decollator heated and stirred the two added with high-speed stirring is dissolved, Heating temperature 60 DEG C.Dissolve the thinner adding 1400ml completely to continue to stir, impel whole solution system viscosity to diminish, be easy to fillers dispersed; Add the conductive filler material flake silver powder 300 grams after sieving after stirring, 6 grams, azepine graphene/nano silver matrix material, after high-speed stirring 5min, add metatitanic acid coupling agent (HY105) 15ml; Continue the organobentonite 15 grams added after high-speed stirring 5min through activation treatment, organic silicon modified by polyether 3 grams, after high-speed stirring 30min, to put into container stand-by as component A for coating.
B component is T31 epoxy curing agent, measures during use by 3% of component A volume, add component A short mix evenly after namely can be used for spraying application.Concrete spray-finishing construction method and method for testing performance are with embodiment 1, and its test-results is in table 1.
Reference examples:
Dimethylbenzene and propyl carbinol by volume 5:4 are hybridly prepared into thinner, measure thinner 491ml, then measure E20 epoxy resin 409ml, and the decollator heated and stirred the two added with high-speed stirring is dissolved, Heating temperature 65 DEG C.Dissolve the thinner adding 1400ml completely to continue to stir, impel whole solution system viscosity to diminish, be easy to fillers dispersed; Add the conductive filler material flake silver powder 400 grams after sieving after stirring, after high-speed stirring 5min, add metatitanic acid coupling agent (HY105) 15ml; Continue the organobentonite 15 grams added after high-speed stirring 5min through activation treatment, after high-speed stirring 30min, to put into container stand-by as component A for coating.
B component is T31 epoxy curing agent, measures during use by 3% of component A volume, add component A short mix evenly after namely can be used for spraying application.Concrete spray-finishing construction method and method for testing performance are with embodiment 1, and its test-results is in table 1.
The performance detection data table of table 1 embodiment and the electromagnetic shielding conductive priming paint prepared by reference examples
The explanation of above embodiment is just for helping related personnel to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement or modification to the present invention, these improve and modification also belongs within the protection domain of the claims in the present invention.

Claims (9)

1. a preparation method for electromagnetic shielding conductive priming paint, is characterized in that: comprise the following steps:
A, use thinner dilution epoxy resin, the decollator heated and stirred then added with high-speed stirring is dissolved;
After b, dissolving completely, then the thinner adding epoxy resin volume 3 ~ 3.5 times continues to stir, and adds conductive filler material, azepine graphene/nanometer metal composite respectively, add coatings additive(s) under high velocity agitation after gained solution stirring is even;
C, continue the organobentonite adding activated process after high-speed stirring, add that quality is solution quality 0.2 ~ 1.5%, and the flow agent of 0.02 ~ 0.5 %, after high-speed stirring, the solution obtained is put into container stand-by as component A;
D, get T31 epoxy curing agent as B component;
B component is measured by 3% of component A volume, for spraying application after short mix is even during use.
2. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, is characterized in that: the epoxy resin wherein in step a is E ~ 20 epoxy resin, and content of epoxy resin is 0.8 to 1 times of diluent volume.
3. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, is characterized in that: wherein thinner by dimethylbenzene and propyl carbinol by volume 5:4 be hybridly prepared into.
4. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, is characterized in that: the conductive filler material wherein in step b is flake silver powder or silver-coated copper powder, and particle diameter is 200 order ~ 250 orders, and its consumption is 10 ~ 30% of solution quality.
5. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, it is characterized in that: the azepine graphene/nanometer metal composite wherein in step b is the one in azepine graphene/nano silver matrix material, azepine graphene/nanometer copper composite material, azepine graphene/nanometer nickel composite material, and its consumption is 0.1 ~ 2% of solution quality.
6. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, is characterized in that: the coatings additive(s) wherein in step b is titanate coupling agent, and its consumption is 0.2 ~ 1.5% of liquor capacity.
7. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, it is characterized in that: the organobentonite of the activated process wherein in step c is through the active process of methyl alcohol sealing, particle diameter is below 200 orders, and its consumption is 0.2 ~ 1.5% of solution quality.
8. the preparation method of electromagnetic shielding conductive priming paint according to claim 1, is characterized in that: the flow agent wherein in step c is the one in organic silicon modified by polyether, polyester resin change properties of organic silicon, and its consumption is solution quality 0.02 ~ 0.5 %.
9. the priming paint prepared by the preparation method of electromagnetic shielding conductive priming paint described in claim 1 ~ 8, is characterized in that: its electric conductivity is less than 0.4 ohm/sheet resistance.
CN201410796032.7A 2014-12-18 2014-12-18 Nitrogen-doped graphene composited electromagnetic shielding type electricity conductive primer and preparation method thereof Pending CN104449239A (en)

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CN104817924A (en) * 2015-03-27 2015-08-05 东莞劲胜精密组件股份有限公司 Graphene modifier, radiation resistant graphene coating and radiation resistant protection film
CN106118387A (en) * 2015-05-08 2016-11-16 台湾奈米碳素股份有限公司 Electromagnetic wave shielding coating
CN106118387B (en) * 2015-05-08 2018-12-11 台湾奈米碳素股份有限公司 Electromagnetic wave shielding coating
CN106189689A (en) * 2016-07-19 2016-12-07 马晓洁 A kind of graphene-based anti-electromagnetic-radiation bicomponent epoxy resin coating
CN108624190A (en) * 2016-07-19 2018-10-09 长泰县石艺建材有限公司 A kind of epoxy coating
CN106493388A (en) * 2016-11-10 2017-03-15 无锡市明盛强力风机有限公司 A kind of preparation method of electromagnetic screen coating filler
JP7090697B2 (en) 2017-06-07 2022-06-24 ルオヤン インスティテュート オブ カッティング-エッジ テクノロジー Electromagnetic wave absorption immersion colloidal solution and electromagnetic wave absorption cellular and its manufacturing method
JP2020521869A (en) * 2017-06-07 2020-07-27 ルオヤン インスティテュート オブ カッティング−エッジ テクノロジーLuoyang Institute Of Cutting−Edge Technology Electromagnetic wave absorption immersion colloidal solution, electromagnetic wave absorption cellular and method of making the same
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CN109354746A (en) * 2018-11-01 2019-02-19 肥西县创玺建材科技有限公司 A kind of plastics with electro-magnetic screen function
CN113121972A (en) * 2019-12-30 2021-07-16 江苏派锐电子有限公司 Novel easy-heat-dissipation anti-aging electronic component plastic shell material
CN115966916A (en) * 2022-12-30 2023-04-14 浙江盛发纺织印染有限公司 Radar wave-absorbing material and production process thereof
CN115966916B (en) * 2022-12-30 2023-08-11 浙江盛发纺织印染有限公司 Radar wave-absorbing material and production process thereof

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Application publication date: 20150325