CN108059863A - A kind of environmental protection electrically-conducting paint and preparation method thereof - Google Patents

A kind of environmental protection electrically-conducting paint and preparation method thereof Download PDF

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CN108059863A
CN108059863A CN201810002821.7A CN201810002821A CN108059863A CN 108059863 A CN108059863 A CN 108059863A CN 201810002821 A CN201810002821 A CN 201810002821A CN 108059863 A CN108059863 A CN 108059863A
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fullerene
conducting paint
environmental protection
preparation
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CN108059863B (en
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许建民
李芳萍
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Guangdong Zhicheng purple light new material Co., Ltd.
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Shandong Dongrui High-Tech Development Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
    • C08F230/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • C09D185/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon; Coating compositions based on derivatives of such polymers
    • C09D185/02—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon; Coating compositions based on derivatives of such polymers containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/085—Copper
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients

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Abstract

The invention discloses a kind of environmentally friendly electrically-conducting paints, are made of following components in parts by weight：60 70 parts of ionomer of fullerene modification film forming, 5 10 parts of copper nanoparticle of silicon-carbon cladding, 38 parts of dispersant.The preparation method of fullerene modification film forming ionomer, including fullerene surface modification, the preparation of copolymer, copolymer grafted, ion exchange.The invention also discloses a kind of preparation methods of the environmentally friendly electrically-conducting paint, include the following steps：Fullerene is modified film forming ionomer, silicon-carbon cladding copper nanoparticle, dispersant to sequentially add high speed mixer in proportion and be uniformly mixed, extruder is added in, in 115 DEG C of meltings of extrusion temperature, is kneaded, cooling, tabletting are crushed through pulverizer, cross 80 mesh sieves, curing 2 days is to get to coating finished product.Environmental protection electrically-conducting paint disclosed by the invention overcomes existing traditional coating filler dispersiveness and poor compatibility, coating adhesion is weak, and metal is oxidized easily, prepare and using when can volatilize harmful substance, it pollutes the environment, the technical issues of health of damage people, wearability, chemical-resistant are poor, thin film and the slow drying speed of constructing.

Description

A kind of environmental protection electrically-conducting paint and preparation method thereof
Technical field
The present invention relates to electrically-conducting paint technical fields more particularly to a kind of environmentally friendly electrically-conducting paint and preparation method thereof.
Background technology
With the development of science and technology, all trades and professions such as oil, chemical industry, medical treatment increasingly tend to mechanization and electronics Change, these factors all cause the harm of electrostatic and electromagnetic radiation pollution in society increasingly domination.Electrostatic is easily in metal And non-metal material surface accumulation, gently then cause the instrument and equipment interruption of service, it is heavy then electronic component will be punctured, cause electric shock, The accidents such as fire or explosion.Electromagenetic wave radiation can not only influence electronic equipment normal use, while can also cause the leakage of information, Can more importantly harm be brought to the health of people.Now, electromagenetic wave radiation oneself become dirty after noise pollution, air The fourth-largest public hazards of human survival safety are threatened after dye, water pollution.Therefore, there is an urgent need for a kind of energy while antistatic and anti-electricity in the industry The technology of magnetic radiation.
At present, the technical method of antistatic and anti-electromagnetic-radiation is more, wherein the use of electrically-conducting paint spraying being a kind of construction Convenient, low-cost method, electrically-conducting paint is with modern science and technology and a kind of features for developing rapidly apply Material, in recent decades, is applied in a variety of military, civilian industrial circles such as electronics, electric appliance, aviation, chemical industry, printing.
Electrically-conducting paint is broadly divided into Intrinsical and addition type, wherein the research on addition type is more.Addition type static conductive Coating is mainly by filling conductive carbon series, metal, metal oxide and macroion etc., these electrically-conducting paints exist at present Greatest problem be dispersiveness and poor compatibility, directly affect the adhesive force of coating, and metal is oxidized easily, and is prepared and is made Used time can volatilize harmful substance, pollute the environment, and damage the health of people, and generally existing wearability, chemically-resistant The technical issues of moral character is poor, thin film and the slow drying speed of constructing.
Therefore, develop one kind and possess superior conductive, antistatic, capability of electromagnetic shielding, weatherability, wearability, antioxygen Change and the environmentally friendly electrically-conducting paint of resistance to UV aging is imperative.
The content of the invention
The goal of the invention of the present invention is to provide a kind of environmentally friendly electrically-conducting paint and preparation method thereof, and the preparation method is simply easy Row, not high to equipment requirement, raw material is easy to get, and convenient post-treatment is cheap, is suitble to large-scale production；The environmental protection being prepared Electrically-conducting paint overcomes existing traditional coating filler dispersiveness and poor compatibility, and coating adhesion is weak, and metal is oxidized easily, Prepare and using when can volatilize harmful substance, pollute the environment, damage the health of people, wearability, chemicals-resistant Property poor, construction film is thin and the technical issues of slow drying speed.
To achieve the above object of the invention, the technical solution adopted by the present invention is：A kind of environmental protection electrically-conducting paint, by following weight The component composition of part：60-70 parts of ionomer of fullerene modification film forming, 5-10 parts of copper nanoparticle of silicon-carbon cladding, dispersant 3-8 Part；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene is scattered in acetone, and adds in 1 thereto, the double (epoxies of 3- Ethane ylmethyl) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones, 30-40 DEG C under oxygen atmosphere Under be stirred to react 5-8 it is small when, after washed 3-5 times with acetone after, solvent is evaporated off in 40-50 DEG C of backspin；
2) preparation of copolymer：Fullerene, 4- vinyl aniline, the 2- for the surface modification that step 1) is prepared will be passed through Methyl -2- 2-hydroxyethyl acrylates phosphate, 4- vinyl benzyl chlorides, vinyltrimethoxysilane are dissolved in high boiling solvent In, after add in initiator thereto, under nitrogen atmosphere, be stirred to react at 55-65 DEG C 2-3 it is small when, after settle out in acetone, and Be placed in 50-60 DEG C of vacuum drying chamber dry 10-15 it is small when；
3) copolymer grafted：The copolymer being prepared by step 2) is dissolved in n,N-Dimethylformamide, then Add in 4,5- dicyano imidazoles thereto, at 40-60 DEG C stir 4-6 it is small when, after settle out in acetone, be placed in 50-60 DEG C Vacuum drying chamber in dry 10-15 it is small when；
4) ion exchange：The mass fraction that the graft copolymer being prepared by step 3) is immersed in 50-60 DEG C is When 30-40 is small in the aqueous solution of four [4- (4'- carboxyl phenyls) phenyl] ethylene of 2-5%, after impregnate 20- in deionized water again 25 it is small when, taking-up be placed in 50-60 DEG C of vacuum drying chamber dry 10-15 it is small when；
Wherein, double (oxiranylmethyl radical) -5- (2- acrylic) of amino modified fullerene, acetone, 1,3- in step 1) - The mass ratio of 1,3,5- triazines -2,4,6 (1H, 3H, 5H)-triketone is (3-5)：(15-25)：(1-2)；
Fullerene, 4- vinyl aniline, the 2- methyl -2- 2-hydroxyethyl acrylates of surface modification described in step 2) Phosphate, 4- vinyl benzyl chlorides, vinyltrimethoxysilane, high boiling solvent, the mass ratio of initiator are 2:1:5:1: 0.5：(15-25)：(0.01-0.03)；
One kind in dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone of the high boiling solvent or It is several；
The initiator is selected from one or more of azodiisobutyronitrile, azobisisoheptonitrile；
Copolymer described in step 3), N,N-dimethylformamide, the mass ratio of 4,5- dicyano imidazoles are (3-5)： (10-15)：(1-2)；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle is added to mass fraction In aqueous isopropanol for the dimethyl polysiloxane of 30-40%, when placement 6-8 is small at 180 DEG C in hydrothermal reaction kettle, take out Reaction kettle is washed repeatedly after reaction system cooling with absolute ethyl alcohol, finally the dry 10- in 50-60 DEG C of vacuum drying chamber 12 it is small when.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
The copper nanoparticle, dimethyl polysiloxane aqueous isopropanol mass ratio be (2-3):10；
The dispersant is selected from one or both of EFKA4046, H-975；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 110-130 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, curing 2 days to get to coating into Product.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
(1) environmentally friendly electrically-conducting paint low in raw material price disclosed by the invention, at low cost, preparation method is simple and practicable, pair sets It is standby of less demanding, it is suitble to large-scale production.
(2) environmentally friendly electrically-conducting paint disclosed by the invention, using the fullerene of surface modification, 4- vinyl aniline, 2- methyl- 2- 2-hydroxyethyl acrylates phosphate, 4- vinyl benzyl chlorides, vinyltrimethoxysilane copolymer form a film as matrix Object, hence it is evident that weatherability, durability and the mechanical property of coating, hydrophily are improved, and adhesive property is strong, rate of drying is fast.
(3) environmentally friendly electrically-conducting paint disclosed by the invention, film forming polymer is Ionomer, is introduced and had by ionic bond There is the anion of conjugated structure, be conducive to improve its electric conductivity.
(4) environmentally friendly electrically-conducting paint disclosed by the invention, the high nano material of introducing this conductivity of fullerene, which is used as, fills out Fill agent, on the one hand, improve its mechanical property and wearability；On the other hand, the electric conductivity of coating is improved；By to fullerene Surface modification is simultaneously grafted with film forming polymer, is conducive to being uniformly dispersed for nano material, by be grafted introduce hydrophilic radical hydroxyl, Amino is conducive to improve its hydrophily.
5) environmentally friendly electrically-conducting paint disclosed by the invention, without the use of organic solvent during use, one reduces cost, and two Harmful substance is not volatilized, it is environmentally protective, be conducive to the health of people.
6) environmentally friendly electrically-conducting paint disclosed by the invention is with the addition of silicon-carbon cladding copper nanoparticle, and fullerene, polyaniline, 4, 5- dicyano imidazoles, four [4- (4'- carboxyl phenyls) phenyl] ethylene units synergistic effect, ensure that coating has more excellent lead Electrically, so as to making it have excellent antistatic, capability of electromagnetic shielding.
7) environmentally friendly electrically-conducting paint disclosed by the invention, copper nanoparticle surface are coated with silicon-carbon, can be prevented that copper from being aoxidized, be improved Paint stability prolongs the service life；It can be bonded with the silicon oxygen bond in film forming polymer molecules chain, uniformly divide so as to improve it The ability of dissipating；And be conducive to improve its resistance to UV aging containing triazine class formation in film forming polymer molecules chain.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
A kind of environmental protection electrically-conducting paint, is made of following components in parts by weight：60 parts of ionomer of fullerene modification film forming, 5 parts of copper nanoparticle of silicon-carbon cladding, 3 parts of dispersant EFKA4046；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene 30g is scattered in acetone 150g, and adds in 1,3- thereto Double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketone 10g, in oxygen atmosphere Be stirred to react at lower 30 DEG C 5 it is small when, after wash 3 times with acetone after, solvent is evaporated off in 40 DEG C of backspins；
2) preparation of copolymer：Fullerene 20g, 4- the vinyl aniline for the surface modification that step 1) is prepared will be passed through 10g, 2- methyl -2- 2-hydroxyethyl acrylate phosphate 50g, 4- vinyl benzyl chlorides 10g, vinyltrimethoxysilane 5g Be dissolved in dimethyl sulfoxide 150g, after add in azodiisobutyronitrile 0.1g thereto, under nitrogen atmosphere, 2 are stirred to react at 55 DEG C Hour, after settle out in acetone, be placed in 50 DEG C of vacuum drying chamber dry 10 it is small when；
3) copolymer grafted：The copolymer 30g being prepared by step 2) is dissolved in N,N-dimethylformamide 100g In, then add in 4,5- dicyano imidazole 10g thereto, at 40 DEG C stir 4 it is small when, after settle out in acetone, be placed in 50 DEG C vacuum drying chamber in dry 10 it is small when；
4) ion exchange：It is 2% by the mass fraction that the graft copolymer being prepared by step 3) is immersed in 50 DEG C Four [4- (4'- carboxyl phenyls) phenyl] ethylene aqueous solution in 40 it is small when, after again in deionized water impregnate 25 it is small when, take out Be placed in 50 DEG C of vacuum drying chamber dry 10 it is small when；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle 20g is added to quality point In aqueous isopropanol 100g of the number for 30% dimethyl polysiloxane, when placement 6 is small at 180 DEG C in hydrothermal reaction kettle, take Go out reaction kettle, washed repeatedly with absolute ethyl alcohol after reaction system cooling, finally drying 10 is small in 50 DEG C of vacuum drying chamber When.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 110 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, and curing 2 days is to get to coating finished product.
Embodiment 2
A kind of environmental protection electrically-conducting paint, is made of following components in parts by weight：63 parts of ionomer of fullerene modification film forming, 7 parts of copper nanoparticle of silicon-carbon cladding, 4 parts of dispersant H-975；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene 35g is scattered in acetone 170g, and adds in 1,3- thereto Double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketone 13g, in oxygen atmosphere Be stirred to react at lower 33 DEG C 6 it is small when, after wash 4 times with acetone after, solvent is evaporated off in 43 DEG C of backspins；
2) preparation of copolymer：Fullerene 20g, 4- the vinyl aniline for the surface modification that step 1) is prepared will be passed through 10g, 2- methyl -2- 2-hydroxyethyl acrylate phosphate 50g, 4- vinyl benzyl chlorides 10g, vinyltrimethoxysilane 5g Be dissolved in n,N-Dimethylformamide 180g, after add in azobisisoheptonitrile 0.15g thereto, under nitrogen atmosphere, at 58 DEG C Be stirred to react 2.4 it is small when, after settle out in acetone, be placed in 52 DEG C of vacuum drying chamber dry 13 it is small when；
3) copolymer grafted：The copolymer 40g being prepared by step 2) is dissolved in N,N-dimethylformamide 130g In, then add in 4,5- dicyano imidazole 14g thereto, at 48 DEG C stir 5 it is small when, after settle out in acetone, be placed in 55 DEG C vacuum drying chamber in dry 13 it is small when；
4) ion exchange：It is 3% by the mass fraction that the graft copolymer being prepared by step 3) is immersed in 53 DEG C Four [4- (4'- carboxyl phenyls) phenyl] ethylene aqueous solution in 34 it is small when, after again in deionized water impregnate 23 it is small when, take out Be placed in 54 DEG C of vacuum drying chamber dry 13 it is small when；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle 25g is added to quality point In aqueous isopropanol 100g of the number for 35% dimethyl polysiloxane, when placement 7 is small at 180 DEG C in hydrothermal reaction kettle, take Go out reaction kettle, washed repeatedly with absolute ethyl alcohol after reaction system cooling, finally drying 11 is small in 54 DEG C of vacuum drying chamber When.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 115 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, and curing 2 days is to get to coating finished product.
Embodiment 3
A kind of environmental protection electrically-conducting paint, is made of following components in parts by weight：66 parts of ionomer of fullerene modification film forming, 7 parts of copper nanoparticle of silicon-carbon cladding, 6 parts of dispersant EFKA4046；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene 43g is scattered in acetone 210g, and adds in 1,3- thereto Double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketone 17g, in oxygen atmosphere Be stirred to react at lower 38 DEG C 7 it is small when, after wash 5 times with acetone after, solvent is evaporated off in 48 DEG C of backspins；
2) preparation of copolymer：Fullerene 20g, 4- the vinyl aniline for the surface modification that step 1) is prepared will be passed through 10g, 2- methyl -2- 2-hydroxyethyl acrylate phosphate 50g, 4- vinyl benzyl chlorides 10g, vinyltrimethoxysilane 5g Be dissolved in, in N-Methyl pyrrolidone 200g, after add in azobisisoheptonitrile 0.2g thereto, under nitrogen atmosphere, stirred at 61 DEG C Mix reaction 2.8 it is small when, after settle out in acetone, be placed in 56 DEG C of vacuum drying chamber dry 14 it is small when；
3) copolymer grafted：The copolymer 40g being prepared by step 2) is dissolved in N,N-dimethylformamide 140g In, then add in 4,5- dicyano imidazole 18g thereto, at 55 DEG C stir 6 it is small when, after settle out in acetone, be placed in 58 DEG C vacuum drying chamber in dry 14 it is small when；
4) ion exchange：It is 4% by the mass fraction that the graft copolymer being prepared by step 3) is immersed in 58 DEG C Four [4- (4'- carboxyl phenyls) phenyl] ethylene aqueous solution in 37 it is small when, after again in deionized water impregnate 24 it is small when, take out Be placed in 58 DEG C of vacuum drying chamber dry 14 it is small when；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle 28g is added to quality point In aqueous isopropanol 100g of the number for 36% dimethyl polysiloxane, when placement 7.5 is small at 180 DEG C in hydrothermal reaction kettle, Reaction kettle is taken out, is washed repeatedly with absolute ethyl alcohol after reaction system cooling, finally dry 12 in 58 DEG C of vacuum drying chamber Hour.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 125 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, and curing 2 days is to get to coating finished product.
Embodiment 4
A kind of environmental protection electrically-conducting paint, is made of following components in parts by weight：68 parts of ionomer of fullerene modification film forming, 9 parts of copper nanoparticle of silicon-carbon cladding, 8 parts of dispersant；The dispersant is EFKA4046, H-975 in mass ratio 3：5 mix；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene 46g is scattered in acetone 230g, and adds in 1,3- thereto Double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketone 19g, in oxygen atmosphere Be stirred to react at lower 39 DEG C 7.8 it is small when, after wash 5 times with acetone after, solvent is evaporated off in 49 DEG C of backspins；
2) preparation of copolymer：Fullerene 20g, 4- the vinyl aniline for the surface modification that step 1) is prepared will be passed through 10g, 2- methyl -2- 2-hydroxyethyl acrylate phosphate 50g, 4- vinyl benzyl chlorides 10g, vinyltrimethoxysilane 5g Be dissolved in dimethyl sulfoxide 240g, after add in azobisisoheptonitrile 0.25g thereto, under nitrogen atmosphere, 3 are stirred to react at 63 DEG C Hour, after settle out in acetone, be placed in 59 DEG C of vacuum drying chamber dry 14 it is small when；
3) copolymer grafted：The copolymer 48g being prepared by step 2) is dissolved in N,N-dimethylformamide 145g In, then add in 4,5- dicyano imidazole 20g thereto, at 59 DEG C stir 6 it is small when, after settle out in acetone, be placed in 59 DEG C vacuum drying chamber in dry 15 it is small when；
4) ion exchange：The mass fraction that the graft copolymer being prepared by step 3) is immersed in 60 DEG C is In the aqueous solution of 4.5% four [4- (4'- carboxyl phenyls) phenyl] ethylene 39 it is small when, after impregnate in deionized water again it is 25 small When, taking-up be placed in 58 DEG C of vacuum drying chamber dry 15 it is small when；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle 29g is added to quality point In aqueous isopropanol 100g of the number for 35% dimethyl polysiloxane, when placement 7.5 is small at 180 DEG C in hydrothermal reaction kettle, Reaction kettle is taken out, is washed repeatedly with absolute ethyl alcohol after reaction system cooling, finally dry 12 in 60 DEG C of vacuum drying chamber Hour.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 128 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, and curing 2 days is to get to coating finished product.
Embodiment 5
A kind of environmental protection electrically-conducting paint, is made of following components in parts by weight：70 parts of ionomer of fullerene modification film forming, 10 parts of copper nanoparticle of silicon-carbon cladding, 8 parts of dispersant EFKA4046；
Wherein, the preparation method of the fullerene modification film forming ionomer, includes the following steps：
1) fullerene surface is modified：Amino modified fullerene 50g is scattered in acetone 250g, and adds in 1,3- thereto Double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketone 20g, in oxygen atmosphere Be stirred to react at lower 40 DEG C 8 it is small when, after wash 5 times with acetone after, solvent is evaporated off in 50 DEG C of backspins；
2) preparation of copolymer：Fullerene 20g, 4- the vinyl aniline for the surface modification that step 1) is prepared will be passed through 10g, 2- methyl -2- 2-hydroxyethyl acrylate phosphate 50g, 4- vinyl benzyl chlorides 10g, vinyltrimethoxysilane 5g Be dissolved in N-Methyl pyrrolidone 250g, after add in azobisisoheptonitrile 0.3g thereto, under nitrogen atmosphere, stirred at 65 DEG C React 3 it is small when, after settle out in acetone, be placed in 60 DEG C of vacuum drying chamber dry 15 it is small when；
3) copolymer grafted：The copolymer 50g being prepared by step 2) is dissolved in N,N-dimethylformamide 150g In, then add in 4,5- dicyano imidazole 20g thereto, at 60 DEG C stir 6 it is small when, after settle out in acetone, be placed in 60 DEG C vacuum drying chamber in dry 15 it is small when；
4) ion exchange：It is 5% by the mass fraction that the graft copolymer being prepared by step 3) is immersed in 60 DEG C Four [4- (4'- carboxyl phenyls) phenyl] ethylene aqueous solution in 40 it is small when, after again in deionized water impregnate 25 it is small when, take out Be placed in 60 DEG C of vacuum drying chamber dry 15 it is small when；
The preparation method of the silicon-carbon cladding copper nanoparticle, includes the following steps：Copper nanoparticle 30g is added to quality point In aqueous isopropanol 100g of the number for 40% dimethyl polysiloxane, when placement 8 is small at 180 DEG C in hydrothermal reaction kettle, take Go out reaction kettle, washed repeatedly with absolute ethyl alcohol after reaction system cooling, finally drying 12 is small in 60 DEG C of vacuum drying chamber When.The product finally obtained calcination 5h under 550 DEG C of nitrogen atmosphere；
A kind of preparation method of the environmentally friendly electrically-conducting paint, includes the following steps：Fullerene is modified into film forming ionic polymerization Object, silicon-carbon cladding copper nanoparticle, dispersant sequentially add high speed mixer and are uniformly mixed in proportion, add in extruder, are squeezing out The melting of 130 DEG C of temperature, is kneaded, and cooling, tabletting is crushed through pulverizer, crosses 80 mesh sieves, and curing 2 days is to get to coating finished product.
Comparative example 2
Commercially available common conductive coating.
Electrically-conducting paint obtained by above-described embodiment 1-5 and comparative example is tested, test result and test method are shown in Table 1。
1 embodiment of table and comparative example coating property
As can be seen from the above table, environmentally friendly electrically-conducting paint disclosed by the embodiments of the present invention, adhesive force 12.5-12.9MPa, surface drying Time is in 8-17min, volume resistivity 7.64 × 106-3.10×106Ω .cm, impact strength 59-74kg.cm, and it is commercially available common Paint adhesion 5.0MPa, surface drying time is in 30min, volume resistivity 4.98 × 108Ω .cm, impact strength 40kg.cm, can See, environmental protection electrically-conducting paint disclosed by the embodiments of the present invention has preferable electric conductivity, adhesive force and impact strength, and drying time Soon.

Claims (10)

1. a kind of environmental protection electrically-conducting paint, it is characterised in that：It is made of following components in parts by weight：Fullerene modification film forming ion gathers Close 60-70 parts of object, 5-10 parts of copper nanoparticle of silicon-carbon cladding, 3-8 parts of dispersant.
2. environmental protection electrically-conducting paint according to claim 1, it is characterised in that：The fullerene modification film forming ionomer Preparation method, include the following steps：
1) fullerene surface is modified：Amino modified fullerene is scattered in acetone, and adds in 1 thereto, the double (ethylene oxide of 3- Ylmethyl) -5- (2- acrylic) -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones stir under oxygen atmosphere at 30-40 DEG C Mix reaction 5-8 it is small when, after washed 3-5 times with acetone after, solvent is evaporated off in 40-50 DEG C of backspin；
2) preparation of copolymer：The fullerene, 4- vinyl aniline, 2- first for the surface modification that step 1) is prepared will be passed through Base -2- 2-hydroxyethyl acrylates phosphate, 4- vinyl benzyl chlorides, vinyltrimethoxysilane are dissolved in high boiling solvent, Add in initiator thereto afterwards, under nitrogen atmosphere, be stirred to react at 55-65 DEG C 2-3 it is small when, after settle out in acetone, juxtaposition When baking 10-15 is small in 50-60 DEG C of vacuum drying chamber；
3) copolymer grafted：The copolymer being prepared by step 2) is dissolved in n,N-Dimethylformamide, then to it Middle addition 4,5- dicyano imidazoles, stirred at 40-60 DEG C 4-6 it is small when, after settle out in acetone, be placed in 50-60 DEG C true When baking 10-15 is small in empty drying box；
4) ion exchange：It is 2-5% by the mass fraction that the graft copolymer being prepared by step 3) is immersed in 50-60 DEG C Four [4- (4'- carboxyl phenyls) phenyl] ethylene aqueous solution in 30-40 it is small when, after again in deionized water impregnate 20-25 it is small When, taking-up be placed in 50-60 DEG C of vacuum drying chamber dry 10-15 it is small when.
3. environmental protection electrically-conducting paint according to claim 2, it is characterised in that：Amino modified fullerene in step 1), acetone, The mass ratio of double (oxiranylmethyl radical) -5- (2- acrylic) -1,3,5- triazines -2,4,6 (1H, 3H, the 5H)-triketones of 1,3- is (3-5)：(15-25)：(1-2).
4. environmental protection electrically-conducting paint according to claim 2, it is characterised in that：The fowler of surface modification described in step 2) Alkene, 4- vinyl aniline, 2- methyl -2- 2-hydroxyethyl acrylates phosphate, 4- vinyl benzyl chlorides, vinyl trimethoxy Silane, high boiling solvent, the mass ratio of initiator are 2:1:5:1:0.5：(15-25)：(0.01-0.03).
5. environmental protection electrically-conducting paint according to claim 2, it is characterised in that：The high boiling solvent be selected from dimethyl sulfoxide, One or more of N,N-dimethylformamide, N-Methyl pyrrolidone；The initiator is selected from azodiisobutyronitrile, azo One or more of two different heptonitriles.
6. environmental protection electrically-conducting paint according to claim 2, it is characterised in that：Copolymer described in step 3), N, N- diformazans Base formamide, the mass ratio of 4,5- dicyano imidazoles are (3-5)：(10-15)：(1-2).
7. environmental protection electrically-conducting paint according to claim 1, it is characterised in that：The preparation side of the silicon-carbon cladding copper nanoparticle Method includes the following steps：Copper nanoparticle is added to the aqueous isopropanol for the dimethyl polysiloxane that mass fraction is 30-40% In, when placement 6-8 is small at 180 DEG C in hydrothermal reaction kettle, reaction kettle is taken out, after reaction system cooling with absolute ethyl alcohol repeatedly Washing, when finally drying 10-12 is small in 50-60 DEG C of vacuum drying chamber.Nitrogen atmosphere of the product finally obtained at 550 DEG C Lower calcination 5h.
8. environmental protection electrically-conducting paint according to claim 7, it is characterised in that：The copper nanoparticle, dimethyl polysiloxane Aqueous isopropanol mass ratio be (2-3):10.
9. environmental protection electrically-conducting paint according to claim 1, it is characterised in that：The dispersant is selected from EFKA4046, H-975 One or both of.
10. environmental protection electrically-conducting paint according to claim 1, it is characterised in that：The preparation method of the environmental protection electrically-conducting paint, Include the following steps：Fullerene is modified film forming ionomer, silicon-carbon cladding copper nanoparticle, dispersant to sequentially add in proportion High speed mixer is uniformly mixed, and adds in extruder, in 110-130 DEG C of melting of extrusion temperature, is kneaded, cooling, tabletting, through pulverizer It crushes, crosses 80 mesh sieves, curing 2 days is to get to coating finished product.
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