CN107142034A - A kind of heat conduction pressure sensitive adhesive and preparation method that graphene is peeled off comprising physics - Google Patents
A kind of heat conduction pressure sensitive adhesive and preparation method that graphene is peeled off comprising physics Download PDFInfo
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- CN107142034A CN107142034A CN201710319552.2A CN201710319552A CN107142034A CN 107142034 A CN107142034 A CN 107142034A CN 201710319552 A CN201710319552 A CN 201710319552A CN 107142034 A CN107142034 A CN 107142034A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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- 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
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/414—Additional features of adhesives in the form of films or foils characterized by the presence of essential components presence of a copolymer
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- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/28—Presence of paper
- C09J2400/283—Presence of paper in the substrate
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Abstract
The present invention discloses a kind of heat conduction pressure sensitive adhesive and preparation method that graphene is peeled off comprising physics, and the composition of pressure sensitive adhesive includes base material, heat conduction adhesive layer, off-style paper layer.Base material lower surface is coated with heat conduction adhesive layer;Prepared heat conduction adhesive layer is composed of the following components:0.4% 1.6% graphenes and 30.4% 49% polyacrylate linear polymers, 50% 68% solvent;Thermal conductive adhesive layer is below off-style paper layer.The present invention is while realization substantially increases thermal conductivity, pressure sensitive adhesive is caused to be provided with preferable initial cohesiveness and hold viscosity energy again, the peel strength and adhesive property with electronic device can be kept for a long time, the stability of heat dispersion is realized, so as to further improve the heat conductivility of pressure sensitive adhesive.
Description
Technical field
The present invention relates to a kind of design and preparation of the pressure sensitive adhesive with heat conductivility, microwave stripping means is based particularly on
Acrylate pressure-sensitive adhesive that the graphene of acquisition and free-radical polymerized method are obtained and the heat conduction pressure sensitive adhesive prepared, belong to heat-conducting glue
Glutinous agent technical field.
Background technology
With the fast development of electronic product, people are particularly ultra-thin to the requirement also more and more higher of portable degree, functionality
The design of panelized, now from mobile phone to computer, volume is less and less, and function is stronger and stronger, is got over which results in integrated level
Come higher, so it is more and more stricter to the cooling requirements of the electronic component on electronic circuit board.Traditional electronic product is used
Fan radiating system, but this system bulk is big, noise is big, be no longer desirable for present electronic product demand and gradually
It is eliminated.Also, simple heat sink material can not effectively play radiating effect to electronic component, and heat conduction pressure sensitive adhesive is pasted
Between electronic component and heat sink material, play a part of connection, barrier between the two can be reduced, effectively improve radiating
Effect.Therefore it is widely used in LCD, semiconductor, in the electronic component such as integrated circuit.With continuing to increase for human demand,
And then other heat sink materials, such as copper foil, aluminium foil are generated, but be due to that this kind of heat sink material is expensive, radiating effect
Production requirement can not be reached, slowly, the new efficient heat sink material of a class occurs in that this kind of material includes carbon fiber, receives
Rice carbon pipe, graphene, diamond film etc..The thermal conductivity of this kind of material is very high, and especially highly-conductive hot carbon fiber axially has
Highest 1200W/mk thermal conductivity, the highest thermal conductivity factor of diamond film is 2200W/mk, and high heat conduction graphene is along flat
Face direction highest 3000-5600W/mk.
Graphene (Graphene) is the sp2 hydridization carbon-coatings of an atom thick, it is tightly packed into bi-dimensional cellular shape knot
Structure[4], it is a kind of two-dimensional material, is the basic architecture unit of the graphite material of every other dimension.It can be warped into zero dimension
Fullerene, is rolled into one-dimensional CNT or is stacked into the graphite of three-dimensional.Graphene has unique carrier properties, in room
Under the conditions of temperature, electron mobility is up to 200000cm2/ VS, can be applied to the field with ballistic electron transport property;Have
Very big specific surface area (2600m2/ g) and higher thermal conductivity (5000W/ (m K);Resistivity very little (about 10-6Ω cm),
Widely used as the minimum material of resistivity in the world;It is that mechanical property is most in the world with unique mechanical characteristic
One of good material, intensity is also harder than steel up to 130GPa, is 100 times of steel.
Graphene can be divided into physics and peel off graphene, redox graphene, modified graphene and graphene oxide.So
And, different types of graphene all has respective advantage and disadvantage, and wherein graphene oxide contains substantial amounts of functional group, therefore can be with
Stable dispersion in organic solvent and can also carry out large-scale production, but substantial amounts of oxygen-containing functional group can cause structure to lack
Fall into, decline its heat conductivility.Modified graphene has good dispersiveness, but its complex manufacturing, and efficiency is low.Reduction-oxidation
Graphene, which equally exists substantial amounts of fault of construction, reduces its heat conductivility., can be big but physics stripping graphene-structured defect is small
Large-scale production, simple production process can effectively improve electrical and thermal conductivity performance.
The content of the invention
The technical problem to be solved in the present invention is the consumption and deployment conditions in a polymer solution for adjusting graphene, gram
Take in graphene composite material because fault of construction between graphene layer and not can be uniformly dispersed in what is caused in polymer
The reduction of heat conductivility, develops new high heat conduction graphene composite film.
A kind of heat conduction polyacrylate pressure-sensitive, it is characterised in that:Including base material, heat conduction adhesive layer, off-style paper layer.Base material
Lower surface is coated with heat conduction adhesive layer;Prepared heat conduction adhesive layer is composed of the following components:0.4%-1.6% graphenes and
30.4%-49% polyacrylate linear polymers, 50%-68% solvent;Thermal conductive adhesive layer is below off-style paper layer.
Further, described base material is cotton paper, PET film, PVA film, PVC film, TAC film or non-woven fabrics.
Further, described polyacrylate linear polymer is obtained by double bond containing acrylic monomer copolymerization, its
It is 20-100 ten thousand to be characterised by molecular weight, and glass transition temperature is -80-50 DEG C.Comonomer used is by following parts by weight
Three kinds or a variety of compositions of component:
5-10 octadecyl acrylate;
5-10 lauryl acrylate;
30-90 hydroxy-ethyl acrylate;
30-90 Isooctyl acrylate monomer;
4-60 butyl acrylate;
4-60 methyl acrylates;
1-5 acrylic acid.
Its preparation method is as follows:
Three kinds used in copolymerization or various of monomer are mixed according to certain ratio, initiator is added and solvent puts into four
In mouth flask, the mass ratio of monomer gross mass used and solvent is 1:1-3, initiator quality used for monomer gross mass 1 ‰-
5%, heating stirring is warming up to 65 DEG C of reaction 5h of certain temperature, then is warming up to 72 DEG C of reaction 2h, then adds initiator and reacts again
2h, the initiator quality added is 1 ‰-the 3% of monomer gross mass, carries out the polyacrylic acid that copolyreaction obtains different molecular weight
Ester linear polymer, whole course of reaction is protected with nitrogen.
Further, the particle diameter of described graphene is 6-35 μm, and the weight/mass percentage composition of carbon is 85-99.5%, the number of plies
For 2-30 layers;
Further, the preparation method of described heat conduction pressure sensitive adhesive is as follows:
Polyacrylate linear polymer, graphene and solvent are mixed according to different proportionings by the method for ultrasonic disperse
Close, enable graphene stable dispersion in a polymer solution.By the graphene polyacrylate mixed solution after ultrasonic disperse
It is coated in bar spreader in release liners, is placed on dry out solvent in baking oven and is then affixed on base material.
Further, the solvent used in the preparation of described polyacrylate linear polymer is ethyl acetate, and toluene is pure
Benzene, dimethylbenzene, 1-METHYLPYRROLIDONE, dioxane, N,N-dimethylformamide, ethanol, methanol, isopropanol, ethylene glycol, four
One or more in hydrogen furans, dichloromethane, chloroform.Expect the polyacrylate polymers of specified molecular weight, then institute
It is 1 with the suitable mass ratio of monomer total amount and solvent:1-3;
Further, described heat conduction pressure sensitive adhesive, it is characterised in that monomer gathers when preparing polyacrylate linear polymer
Initiator needed for closing is azodiisobutyronitrile, ABVN, azo-bis-isobutyrate hydrochloride, di-tert-butyl peroxide
One or more in thing, persulfate, benzoyl peroxide, peroxidized t-butyl perbenzoate, diisopropyl peroxide carbonate,
Initiator quality is 1 ‰-the 5% of monomer gross mass, the initiator quality added in course of reaction for monomer gross mass 1 ‰-
3%;
Further, the optimal thickness of the base material used in described heat conduction pressure sensitive adhesive is 10-100 μm, is not influenceing pressure
The optimum thickness of adhesive layer is 20-100 μm on the premise of quick colloidality energy;
Further, the preparation of described heat conduction pressure sensitive adhesive uses the high speed that rate of dispersion is 2000-3000r/min
Scattered and ultrasonic power is 300-800W, and frequency is the scattered method of 2000-3000Hz high frequency ultrasound.
The advantageous effects of the present invention:
(1) the heat conduction pressure sensitive adhesive prepared using the method for the invention is not influenceing pressure sensitive adhesive itself initial bonding strength, holding power
With heat-conducting effect can be effectively improved on the premise of peel strength performance.
(2) the method for the invention technique is simple, and heat filling graphene phosphorus content used is high, and defect is few, Ke Yiwen
It is fixed to disperse in the polymer.
(3) conventional graphene heat conduction pressure sensitive adhesive is that graphene layer is directly composited with base material by adhesive layer.And
Heat conduction pressure sensitive adhesive of the present invention is prepared by the directly method that mixes graphene with adhesive, and the method can be by stone
Black alkene is dispersed in a polymer solution, can effectively improve thermal conductivity.
(4) the heat conduction pressure sensitive adhesive that is prepared with graphene is heat filling of the present invention with by metal material (metal from
Son), nonmetallic materials (graphite, carbon black, CNT), high heat conduction filler (the metal powder class such as Al, Cu, Ag filler), metal oxygen
The heat conduction pressure sensitive adhesive phase of the preparations such as compound class filler (Al2O3, MgO etc.), nonmetallic heat conductive filler (SiC, AIN, Si3N4 etc.)
Than the characteristics of with being uniformly dispersed, the heat conductivility of pressure sensitive adhesive most importantly can be effectively improved.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to
Limit the present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiied
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also understand the present invention completely.What the number in following examples was not particularly illustrated is mass fraction.
Embodiment 1
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 39.6 parts of molecular weight be 400,000 polyacrylate linear polymer in 30 parts of ethyl acetate.Take 0.4
Part particle diameter is 6 μm, and carbon content is 99.5%, and the number of plies is added to 30 parts of ethyl acetate for 2-30 layers of physics stripping graphene powder
Medium-high frequency ultrasound 2min, frequency is 2000Hz, ultrasonic power 300W.By the ethyl acetate solution and high frequency ultrasound of polyacrylate
Graphene organic solution afterwards mixes again, rate of dispersion 2000r/min, jitter time scattered with high speed dispersor
30min.Finely dispersed mixed solution is coated uniformly in release liners, coating thickness is 60 μm, is then 10 μm with thickness
PET film be covered in the test that various performances are carried out in adhesive layer.
Embodiment 2
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 49 parts of molecular weight be 400,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.It is 6 to take 1 part of particle diameter
μm, carbon content is 99.5%, and the number of plies is that 2-30 layers of physics stripping graphene powder are added to 25 parts of ethyl acetate high frequency ultrasounds
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 20 μm, is then covered in glue with thickness for 10 μm of PET film
The test of various performances is carried out on glutinous layer.
Embodiment 3
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 30.4 parts of molecular weight be 400,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 6 μm, and carbon content is 99.5%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 10 μm of PET film
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 4
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 39.6 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 30 parts of ethyl acetate.Take 0.4 part of grain
Footpath is 6 μm, and carbon content is 99.5%, and the number of plies is added to 30 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 2000Hz, ultrasonic power 300W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 2000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 60 μm, is then pasted for 50 μm of PVA film with thickness
The test of various performances is carried out in adhesive layer.
Embodiment 5
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 49 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.It is 6 to take 1 part of particle diameter
μm, carbon content is 99.5%, and the number of plies is added to 25 parts of ethyl acetate high frequency ultrasounds for 2-30 layers of physics stripping graphene powder
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 20 μm, is then covered in glue with thickness for 50 μm of PVA film
The test of various performances is carried out on glutinous layer.
Embodiment 6
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 30.4 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 6 μm, and carbon content is 99.5%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 50 μm of PVA film
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 7
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 39.6 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 30 parts of ethyl acetate.Take 0.4 part of grain
Footpath is 6 μm, and carbon content is 99.5%, and the number of plies is added to 30 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 2000Hz, ultrasonic power 300W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 2000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 60 μm, then pasted with thickness for 100 μm of PVC film
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 8
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 49 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.It is 6 to take 1 part of particle diameter
μm, carbon content is 99.5%, and the number of plies is added to 25 parts of ethyl acetate high frequency ultrasounds for 2-30 layers of physics stripping graphene powder
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 20 μm, is then covered in thickness for 100 μm of PVC film
The test of various performances is carried out in adhesive layer.
Embodiment 9
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 30.4 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 6 μm, and carbon content is 99.5%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 100 μm of PVC film
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 10
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 39.6 parts of molecular weight be 400,000 polyacrylate linear polymer in 30 parts of ethyl acetate.Take 0.4
Part particle diameter is 35 μm, and carbon content is 85%, and the number of plies is added to 30 parts of ethyl acetate for 2-30 layers of physics stripping graphene powder
Medium-high frequency ultrasound 2min, frequency is 2000Hz, ultrasonic power 300W.By the ethyl acetate solution and high frequency ultrasound of polyacrylate
Graphene organic solution afterwards mixes again, rate of dispersion 2000r/min, jitter time scattered with high speed dispersor
30min.Finely dispersed mixed solution is coated uniformly in release liners, coating thickness is 60 μm, is then 10 μm with thickness
TVC films be covered in the test that various performances are carried out in adhesive layer.
Embodiment 11
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 49 parts of molecular weight be 400,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.1 part of particle diameter is taken to be
35 μm, carbon content is 85%, and the number of plies is added to 25 parts of ethyl acetate high frequency ultrasounds for 2-30 layers of physics stripping graphene powder
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 40 μm, is then covered in glue with thickness for 10 μm of TVC films
The test of various performances is carried out on glutinous layer.
Embodiment 12
5 parts of lauryl acrylates are taken, 90 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid are added in four-hole boiling flask, then added
5 parts of initiator benzoyl peroxides and 200 parts of solvent toluenes, heating stirring are warming up to 65 DEG C of reaction 5h, then are warming up to 72 DEG C instead
2h is answered, 1 part of initiator benzoyl peroxide is then added and reacts 2h again, it is 400,000, glass to carry out copolyreaction and obtain molecular weight
Change the polyacrylate linear polymer that transition temperature is -50 DEG C, whole course of reaction is protected with nitrogen.
Weigh 30.4 parts of molecular weight be 400,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 35 μm, and carbon content is 85%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 10 μm of TVC films
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 13
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 39.6 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 30 parts of ethyl acetate.Take 0.4 part of grain
Footpath is 35 μm, and carbon content is 85%, and the number of plies is added to 30 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 2000Hz, ultrasonic power 300W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 2000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 60 μm, then pasted with thickness for 50 μm of non-woven fabrics
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 14
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 49 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.1 part of particle diameter is taken to be
35 μm, carbon content is 85%, and the number of plies is added to 25 parts of ethyl acetate high frequency ultrasounds for 2-30 layers of physics stripping graphene powder
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 20 μm, is then covered in thickness for 50 μm of non-woven fabrics
The test of various performances is carried out in adhesive layer.
Embodiment 15
5 parts of octadecyl acrylates are taken, 50 parts of Isooctyl acrylate monomers, 44 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 4 parts of initiator azodiisobutyronitriles and 150 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 2 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 500,000 to molecular weight, glass transition temperature is -40 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 30.4 parts of molecular weight be 500,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 35 μm, and carbon content is 85%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 50 μm of non-woven fabrics
Overlay in adhesive layer and carry out the test of various performances.
Embodiment 16
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 39.6 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 30 parts of ethyl acetate.Take 0.4 part of grain
Footpath is 35 μm, and carbon content is 85%, and the number of plies is added to 30 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 2000Hz, ultrasonic power 300W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 2000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 60 μm, is then pasted for 100 μm of cotton paper with thickness
The test of various performances is carried out in adhesive layer.
Embodiment 17
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 49 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 25 parts of ethyl acetate.1 part of particle diameter is taken to be
35 μm, carbon content is 85%, and the number of plies is added to 25 parts of ethyl acetate high frequency ultrasounds for 2-30 layers of physics stripping graphene powder
2min, frequency is 2500Hz, ultrasonic power 500W.By the graphene after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Organic solution mixes again, rate of dispersion 2500r/min, jitter time 30min scattered with high speed dispersor.Will be scattered equal
Even mixed solution is coated uniformly in release liners, and coating thickness is 20 μm, is then covered in glue with thickness for 100 μm of cotton paper
The test of various performances is carried out on glutinous layer.
Embodiment 18
5 parts of octadecyl acrylates are taken, 80 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates, 1 part of acrylic acid is added to four mouthfuls
In flask, 3 parts of initiator azodiisobutyronitriles and 100 parts of solvent ethyl acetates are then added, heating stirring is warming up to 65 DEG C instead
5h is answered, then is warming up to 72 DEG C of reaction 2h, 3 parts of initiator azodiisobutyronitriles is then added and reacts 2h again, carry out copolyreaction and obtain
It is 600,000 to molecular weight, glass transition temperature is -20 DEG C of polyacrylate linear polymer, whole course of reaction nitrogen
Protection.
Weigh 30.4 parts of molecular weight be 600,000 polyacrylate pressure-sensitive in 34 parts of ethyl acetate.Take 1.6 parts of grains
Footpath is 35 μm, and carbon content is 85%, and the number of plies is added to 34 parts of ethyl acetate high frequencies for 2-30 layers of physics stripping graphene powder
Ultrasonic 2min, frequency is 3000Hz, ultrasonic power 800W.By the stone after the ethyl acetate solution and high frequency ultrasound of polyacrylate
Black alkene organic solution mixes again, rate of dispersion 3000r/min, jitter time 30min scattered with high speed dispersor.It will divide
Dissipate uniform mixed solution to be coated uniformly in release liners, coating thickness is 100 μm, then pasted with thickness for 100 μm of cotton paper
Overlay in adhesive layer and carry out the test of various performances.
Initial bonding strength selects GB4852-02 standard testing initial bonding strengths using CZY-G type initial bonding strengths tester.
Holding power selects GB4851-98 standard testing holding powers using CZY-6S type holding powers tester.
Peel strength selects GB2792-98 standard testing pressures using BLD-200N type 180 degree adhesive tapes peeling strength testing machine
Peel strength of the quick glue on glass.
Thermal conductivity uses the horizontal thermal conductivity of ASTM D7984 standard testing films using C-THERM TCI instruments.
Table 1 is initial bonding strength, holding power, peel strength and the thermal conductivity data of each embodiment final products
Claims (9)
1. a kind of heat conduction polyacrylate pressure-sensitive, it is characterised in that:Including base material, heat conduction adhesive layer, off-style paper layer;Base material
Thickness is 10-100 μm;The thickness of heat conduction adhesive layer is 20-100 μm;Base material lower surface is coated with heat conduction adhesive layer;Prepared
Heat conduction adhesive layer is composed of the following components:0.4%-1.6% graphenes and 30.4%-49% polyacrylate linear polymers,
50%-68% solvent;Thermal conductive adhesive layer is below off-style paper layer.
2. a kind of heat conduction polyacrylate pressure-sensitive according to claim 1, it is characterised in that:Base material is cotton paper, PET
Film, PVA film, PVC film, TAC film or non-woven fabrics.
3. a kind of heat conduction polyacrylate pressure-sensitive according to claim 1, it is characterised in that:Polyacrylate linearly gathers
Compound is obtained by double bond containing acrylic monomer copolymerization, and molecular weight is 20-100 ten thousand, and glass transition temperature is-80-50
℃;Three kind compositions of the comonomer at least including following parts by weight of component:
5-10 octadecyl acrylate;
5-10 lauryl acrylate;
30-90 hydroxy-ethyl acrylate;
30-90 Isooctyl acrylate monomer;
4-60 butyl acrylate;
4-60 methyl acrylates;
1-5 acrylic acid.
4. a kind of heat conduction polyacrylate pressure-sensitive according to claim 1-3 any one, it is characterised in that:Described
Polyacrylate linear polymer preparation method is as follows:
Three kinds or more monomer used in copolymerization is mixed, initiator is added and solvent is put into four-hole boiling flask, it is used
The mass ratio of monomer gross mass and solvent is 1:1-3, initiator quality used is 1 ‰-the 5% of monomer gross mass, heating stirring
65 DEG C of reaction 5h are warming up to, then are warming up to 72 DEG C of reaction 2h, initiator are then added, the initiator quality added is the total matter of monomer
1 ‰-the 3% of amount, then 2h is reacted, the polyacrylate linear polymer that copolyreaction obtains different molecular weight is carried out, it is whole anti-
Process is answered to be protected with nitrogen.
5. a kind of heat conduction polyacrylate pressure-sensitive according to claim 4, it is characterised in that:Prepare polyacrylate line
Property polymer when the solvent that adds be ethyl acetate, toluene, purified petroleum benzin, dimethylbenzene, 1-METHYLPYRROLIDONE, dioxane, N, N-
One or more in dimethylformamide, ethanol, methanol, isopropanol, ethylene glycol, tetrahydrofuran, dichloromethane, chloroform.
6. a kind of heat conduction polyacrylate pressure-sensitive according to claim 4, it is characterised in that:Prepare polyacrylate line
Property polymer when monomer polymerization needed for initiator be azodiisobutyronitrile, ABVN, azo-bis-isobutyrate hydrochloride,
Di-tert-butyl peroxide, persulfate, benzoyl peroxide, peroxidized t-butyl perbenzoate, diisopropyl peroxide carbonate
In one or more.
7. a kind of heat conduction polyacrylate pressure-sensitive according to claim 1, it is characterised in that:The particle diameter of graphene is 6-
35 μm, carbon weight/mass percentage composition is 85-99.5%, and the number of plies is 2-30 layers.
8. prepare a kind of heat conduction polyacrylate pressure-sensitive as described in claim 1-7 any one, it is characterised in that:
Polyacrylate linear polymer, graphene and solvent are mixed according to different proportionings by the method for ultrasonic disperse,
Enable graphene stable dispersion in the polymer;Graphene polyacrylate mixed solution after ultrasonic disperse is applied with bar
Cloth device is coated in release liners, is placed on dry out solvent in baking oven and is then affixed on base material.
9. according to the method described in claim 1, it is characterised in that:The preparation of thermal conductive adhesive uses scattered and high at a high speed
The method of frequency ultrasonic disperse;Ultrasonic power is 300-800W, and frequency is 2000-3000Hz, and rate of dispersion is 2000-3000r/
min。
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