CN107312483A - A kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof - Google Patents

A kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof Download PDF

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CN107312483A
CN107312483A CN201710658835.XA CN201710658835A CN107312483A CN 107312483 A CN107312483 A CN 107312483A CN 201710658835 A CN201710658835 A CN 201710658835A CN 107312483 A CN107312483 A CN 107312483A
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epoxy resins
heat conduction
aqueous epoxy
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陈东进
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Dongguan Lianzhou Intellectual Property Operation and Management 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
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • 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
    • 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
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • 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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof, in parts by weight, including following components：100 parts of bisphenol A type epoxy resin, 50 60 parts of sodium alginate, 30 48 parts of composite heat-conducting particle, 20 40 parts of polyethylene glycol 200,9 14 parts of DMP, 11 19 parts of ethylhydroxyethylcellulose, 69 parts of surfactant, 57 parts of toughener, 36 parts of coupling agent, 20 27 parts of curing agent, 30 60 parts of water.The thermal conductive adhesive of the application has good heat-conducting effect, and heat transfer efficiency is high, and adhesive property is good, and it still is able to keep under the high temperature conditions good stability.

Description

A kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof
Technical field
The present invention relates to textile auxiliary field, more particularly to a kind of aqueous epoxy resins type heat conduction adhesive and its preparation Method.
Background technology
With the development of science and technology, people for electronic product requirement more and more higher, electronic product forward direction miniaturization, The direction of slimming, cost degradation and multifunction is developed.The thermal diffusion problem of integrated circuit and electronic component into For electronic industry it is most important the problem of, the development of the performance, speed of microelectronic product further to minimize can be limited.Height is led Heat, high thermal stability, the heat conductive insulating encapsulating material of environmental protection have become the new demand of electronic industry, and this leads to traditional electronics Hot encapsulation material proposes new challenge.Traditional coloring material：Such as copper, aluminium, inorganic ceramic material conducts heat rate are higher, are leading The radiating requirements of electronic product can be met in hot property, but there is higher density, processing difficulties, electrical insulating property in this kind of material Can not be good, the shortcoming with electronic product adhesive property difference, it is difficult to reach existing technical requirements.Therefore, with electronic product Continue to develop, exploitation Novel heat dissipation material turns into urgent problem to be solved.
The research to heat conduction adhesive is broadly divided into two kinds of directions at present：One kind is to prepare Intrinsical heat conduction adhesive, i.e., It is by changing polymer molecule or link structure so that polymer molecule can effectively conduct heat energy；Another is to prepare Filled-type thermally conductive adhesive, is by adding high heat conduction material in the not good high polymer material of heat conductivility, so as to realize Composite has higher heat conductivility.Intrinsical heat conduction adhesive stability is good, and structure is affected by environment smaller, but adds Work complex process, it is difficult to accomplish scale production, and filled-type thermally conductive gluing agent producing process is relatively simple, less-restrictive, because This is of great interest.
Epoxy resin is referred to containing two or more epoxy radicals, organic with alicyclic, aromatic series or aliphatic etc. Compound is skeleton, and the sub- oligomer that can be secured satisfactory grades by epoxide group reaction.Epoxy resin belongs to thermosetting resin, Under the conditions of 120 DEG C of the curing agent existence conditions such as anhydrides, aromatic amine, polyphenol, alicyclic, dicyandiamide and isocyanates Solidification.The solidification of epoxy resin relies primarily on the ring opening polyaddition of epoxy radicals, passes through open loop -ester-etherificate constantly repeatedly Course of reaction is realized.
Chinese patent CN201010570659.2 discloses a kind of high temperature resistance high heat conduction glue, and the colloid is main by asphalt mixtures modified by epoxy resin Fat, curing agent, curing accelerator and high heat conduction filler composition；Epoxy resin is cycloaliphatic epoxy resin, and curing agent is that hexahydro is adjacent Phthalate anhydride, curing accelerator is modified amine accelerator, and high heat conduction filler is nano aluminum nitride (AlN) whisker, nanometer nitrogen Change boron (BN) powder or nano aluminum nitride powder.The invention also provides the preparation method of above high temperature resistance high heat conduction glue, the side Method is：Curing agent and curing accelerator are dispersed in epoxy resin, after then being mixed with high heat conduction filler, grinding is used Machine grinding is uniform.After tested, the high temperature resistance high heat conduction adhesive curing thing glass transition temperature is higher than 150 DEG C；Adhesion strength is reachable To more than 16Mpa, and after 260 DEG C of temperature bakings, adhesion strength reduction is no more than 5%；Thermal conductivity factor can reach 4.0W/m K。
The content of the invention
It is an object of the invention to provide a kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof, the heat conduction is gluing Agent has good heat-conducting effect, and heat transfer efficiency is high, and adhesive property is good, and it still is able to keep well under the high temperature conditions Stability.
To achieve the above object, the present invention uses following technical scheme：
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 50-60 parts of sodium alginate, 30-48 parts of composite heat-conducting particle, polyethylene glycol -200 20-40 parts, 9-14 parts of DMP, 11-19 parts of ethylhydroxyethylcellulose, 6-9 parts of surfactant, 5-7 parts of toughener, coupling agent 3-6 parts, 20-27 parts of curing agent, 30-60 parts of water；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, Add nano-TiO2Powder and nano boron nitride powder, the ultrasonic disperse 1-2h under the conditions of 70-80 DEG C, afterwards in 70-80 DEG C of bar It is stirred vigorously under part, NaOH and Na is added dropwise into mixture2CO3Mixed solution, after being added dropwise to complete continue stir 90-120min, It is stood to 36h under the conditions of 70-80 DEG C after stopping stirring, filters, wash afterwards, dry obtained-TiMgAl houghites are answered Close heat conduction particle.
It is preferred that, Mg, Al, Ti mol ratio are 9 in the composite heat-conducting particle:3:1.
It is preferred that, the mass ratio in the composite heat-conducting particle shared by BN is 63%-79%.
It is preferred that, the addition and nitre of dodecyl dihydroxy ethyl glycine betaine in the preparation method of the composite heat-conducting particle The mass ratio of sour magnesium is 1：40.
It is preferred that, the surfactant is the mixed of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone Compound.
It is preferred that, the toughener is the mixture of ABS rubber and ethylene-methyl acrylate copolymer.
It is preferred that, the coupling agent is titanate coupling agent.
It is preferred that, the curing agent is the mixture of beta-hydroxyethyl ethylenediamine and diethylenetriamine.
A kind of preparation method of aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 45-60min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 30-45min, be afterwards put into composite heat-conducting particle powder In the aqueous solution of coupling agent, regulation pH is 3-5, carries out ultrasonic disperse 40-60min, adds polyethylene glycol -200 and stirs, it Mixed emulsion, DMP, ethylhydroxyethylcellulose, the toughener afterwards prepared by step (1) is added thereto, and it is 80-90 to control temperature DEG C, it is uniformly mixed, is down to room temperature, is afterwards added thereto curing agent, is well mixed, produces the aqueous epoxy resins type Heat conduction adhesive.
The invention has the advantages that,
The application prepares hydrotalcite-like composite material using nm-class boron nitride and nano titanium oxide as core.Using nanometer The heat conduction particle that boron nitride is prepared with the mode that houghite is combined, while with good heat-conducting effect, class neatly Stone structure after preheat can deviate from the moisture in its structure, so as to improve cooling rate, improve heat transfer efficiency.Sodium alginate is A kind of natural material, it is used cooperatively with bisphenol A type epoxy resin, and can effectively improve adhesive coheres effect, carries Height coheres fastness.
Embodiment
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 50 parts of sodium alginate, 30 parts of composite heat-conducting particle, 20 parts of polyethylene glycol -200, 9 parts of DMP, 11 parts of ethylhydroxyethylcellulose, 6 parts of surfactant, 5 parts of toughener, 3 parts of coupling agent, 20 parts of curing agent, water 30 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 1h under the conditions of 70 DEG C is stirred vigorously under the conditions of 70 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 90min, stop stirring after it is stood into 36h under the conditions of 70 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 63%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 45min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 30min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 3, carries out ultrasonic disperse 40min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 80 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
Embodiment 2
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 60 parts of sodium alginate, 48 parts of composite heat-conducting particle, 40 parts of polyethylene glycol -200, 14 parts of DMP, 19 parts of ethylhydroxyethylcellulose, 9 parts of surfactant, 7 parts of toughener, 6 parts of coupling agent, 27 parts of curing agent, water 60 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 2h under the conditions of 80 DEG C is stirred vigorously under the conditions of 80 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 120min, stop stirring after it is stood into 36h under the conditions of 80 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 79%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 60min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 45min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 5, carries out ultrasonic disperse 60min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 90 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
Embodiment 3
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 50 parts of sodium alginate, 48 parts of composite heat-conducting particle, 20 parts of polyethylene glycol -200, 14 parts of DMP, 11 parts of ethylhydroxyethylcellulose, 9 parts of surfactant, 5 parts of toughener, 6 parts of coupling agent, 20 parts of curing agent, water 60 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 2h under the conditions of 70 DEG C is stirred vigorously under the conditions of 70 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 120min, stop stirring after it is stood into 36h under the conditions of 70 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 79%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 45min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 45min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 3, carries out ultrasonic disperse 60min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 80 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
Embodiment 4
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 60 parts of sodium alginate, 30 parts of composite heat-conducting particle, 40 parts of polyethylene glycol -200, 9 parts of DMP, 19 parts of ethylhydroxyethylcellulose, 6 parts of surfactant, 7 parts of toughener, 3 parts of coupling agent, 27 parts of curing agent, water 30 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 1h under the conditions of 80 DEG C is stirred vigorously under the conditions of 80 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 90min, stop stirring after it is stood into 36h under the conditions of 80 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 63%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 60min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 30min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 5, carries out ultrasonic disperse 40min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 90 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
Embodiment 5
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 52 parts of sodium alginate, 32 parts of composite heat-conducting particle, 28 parts of polyethylene glycol -200, DMP11 parts, 13 parts of ethylhydroxyethylcellulose, 7 parts of surfactant, 6 parts of toughener, 4 parts of coupling agent, 22 parts of curing agent, water 40 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 1h under the conditions of 80 DEG C is stirred vigorously under the conditions of 80 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 90min, stop stirring after it is stood into 36h under the conditions of 80 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 69%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 60min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 30min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 5, carries out ultrasonic disperse 40min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 90 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
Embodiment 6
A kind of aqueous epoxy resins type heat conduction adhesive, in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 57 parts of sodium alginate, 42 parts of composite heat-conducting particle, -20034 parts of polyethylene glycol, DMP12 parts, 17 parts of ethylhydroxyethylcellulose, 8 parts of surfactant, 6 parts of toughener, 5 parts of coupling agent, 24 parts of curing agent, water 50 parts；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, The addition of dodecyl dihydroxy ethyl glycine betaine and the mass ratio of magnesium nitrate are 1：40, add nano-TiO2Powder and nanometer nitrogen Change boron powder, the ultrasonic disperse 2h under the conditions of 80 DEG C is stirred vigorously under the conditions of 80 DEG C afterwards, be added dropwise into mixture NaOH and Na2CO3Mixed solution, after being added dropwise to complete continue stir 120min, stop stirring after it is stood into 36h under the conditions of 80 DEG C, it Filter, wash afterwards, drying obtained-TiMgAl houghite composite heat-conducting particles；Mg, Al, Ti mole in composite heat-conducting particle Than for 9:3:1；Mass ratio in composite heat-conducting particle shared by BN is 74%.
Surfactant is the mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone；Toughener For ABS rubber and the mixture of ethylene-methyl acrylate copolymer；Coupling agent is titanate coupling agent；Curing agent is β-hydroxyl second The mixture of base ethylenediamine and diethylenetriamine.
The preparation method of the aqueous epoxy resins type heat conduction adhesive, is comprised the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, is added into afterwards in the aqueous solution of surfactant, It is well mixed, sodium alginate stirring 50min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 40min, composite heat-conducting particle powder is put into idol afterwards In the aqueous solution for joining agent, regulation pH is 4, carries out ultrasonic disperse 50min, adds polyethylene glycol -200 and stirs, afterwards will step Suddenly the mixed emulsion, DMP, ethylhydroxyethylcellulose, toughener of (1) preparation are added thereto, and it is 90 DEG C to control temperature, and stirring is mixed Close uniform, be down to room temperature, be afterwards added thereto curing agent, be well mixed, produce the aqueous epoxy resins type heat conduction gluing Agent.
The heat conductivility of the embodiment 1-6 aqueous epoxy resins type heat conduction adhesives prepared and comparative example is tested, As a result as in the table below：
Thermal conductivity tests the thermal conductivity factor of measured material by heat flow method conductometer, and thermal conductivity factor is higher to show thermal conductivity more It is good.
Comparative example is commercially available aqueous epoxy resins type heat conduction adhesive.
As can be seen here, the heat conduction adhesive thermal conductivity factor that prepared by the embodiment of the present application 1-6 is superior to comparative example, the application institute The thermal conductive adhesive stated has good heat conductivility and thermal stability.

Claims (9)

1. a kind of aqueous epoxy resins type heat conduction adhesive, it is characterised in that in parts by weight, including following components：
100 parts of bisphenol A type epoxy resin, 50-60 parts of sodium alginate, 30-48 parts of composite heat-conducting particle, the 20- of polyethylene glycol -200 40 parts, 9-14 parts of DMP, 11-19 parts of ethylhydroxyethylcellulose, 6-9 parts of surfactant, 5-7 parts of toughener, coupling agent 3-6 Part, 20-27 parts of curing agent, 30-60 parts of water；
The preparation method of the composite heat-conducting particle is：
Magnesium nitrate, aluminum nitrate are dissolved in the water, after addition dodecyl dihydroxy ethyl glycine betaine stirs thereto, added Nano-TiO2Powder and nano boron nitride powder, the ultrasonic disperse 1-2h under the conditions of 70-80 DEG C, afterwards under the conditions of 70-80 DEG C It is stirred vigorously, NaOH and Na is added dropwise into mixture2CO3Mixed solution, after being added dropwise to complete continue stir 90-120min, stop It is stood to 36h after stirring under the conditions of 70-80 DEG C, filters, wash afterwards, drying obtained-TiMgAl houghite composite guides Hot particle.
2. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The composite heat-conducting particle Middle Mg, Al, Ti mol ratio are 9:3:1.
3. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The composite heat-conducting particle Mass ratio shared by middle BN is 63%-79%.
4. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The composite heat-conducting particle Preparation method in dodecyl dihydroxy ethyl glycine betaine addition and magnesium nitrate mass ratio be 1：40.
5. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The surfactant is The mixture of coconut oleoyl monoethanolamine and dodecanamide propyl decil lactone.
6. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The toughener is ABS The mixture of rubber and ethylene-methyl acrylate copolymer.
7. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The coupling agent is metatitanic acid Ester coupling agent.
8. aqueous epoxy resins type heat conduction adhesive according to claim 1, it is characterised in that：The curing agent is β-hydroxyl The mixture of ethylethylenediamine and diethylenetriamine.
9. the preparation method of the aqueous epoxy resins type heat conduction adhesive according to claim any one of 1-8, its feature exists In comprising the steps of：
(1) bisphenol A type epoxy resin is crushed using colloid mill, be added into afterwards in the aqueous solution of surfactant, mixed Uniformly, sodium alginate stirring 45-60min is added, mixed emulsion is made；
(2) composite heat-conducting particle is put into ball mill, grinds 30-45min, composite heat-conducting particle powder is put into coupling afterwards In the aqueous solution of agent, regulation pH is 3-5, carries out ultrasonic disperse 40-60min, adds polyethylene glycol -200 and stirs, and afterwards will Mixed emulsion, DMP, ethylhydroxyethylcellulose, the toughener of step (1) preparation are added thereto, and it is 80-90 DEG C to control temperature, It is uniformly mixed, is down to room temperature, is afterwards added thereto curing agent, is well mixed, produces the aqueous epoxy resins type and lead Hot adhesive.
CN201710658835.XA 2017-08-04 2017-08-04 A kind of aqueous epoxy resins type heat conduction adhesive and preparation method thereof Withdrawn CN107312483A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108219729A (en) * 2018-01-19 2018-06-29 中国石油天然气股份有限公司 A kind of artificial rock core adhesive
CN109403574A (en) * 2018-12-15 2019-03-01 景泰县金龙化工建材有限公司 A kind of acoustical gypsum board and preparation method thereof
CN111876115A (en) * 2020-08-18 2020-11-03 上海澳昌实业有限公司 Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof
CN115820082A (en) * 2022-11-24 2023-03-21 国网浙江省电力有限公司超高压分公司 Thermosensitive color-changing temperature-indicating coating and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110284160A1 (en) * 2010-05-18 2011-11-24 Cognis Ip Management Gmbh 2-Component Adhesives
CN103228753A (en) * 2010-12-01 2013-07-31 东丽株式会社 Adhesive composition, adhesive sheet, and semiconductor device using the adhesive composition or the adhesive sheet
CN104449448A (en) * 2014-11-27 2015-03-25 昆山汉品电子有限公司 Metal-substrate double-matte-surface electrically-conductive carbon composite material and processing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110284160A1 (en) * 2010-05-18 2011-11-24 Cognis Ip Management Gmbh 2-Component Adhesives
CN103228753A (en) * 2010-12-01 2013-07-31 东丽株式会社 Adhesive composition, adhesive sheet, and semiconductor device using the adhesive composition or the adhesive sheet
CN104449448A (en) * 2014-11-27 2015-03-25 昆山汉品电子有限公司 Metal-substrate double-matte-surface electrically-conductive carbon composite material and processing method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108219729A (en) * 2018-01-19 2018-06-29 中国石油天然气股份有限公司 A kind of artificial rock core adhesive
CN109403574A (en) * 2018-12-15 2019-03-01 景泰县金龙化工建材有限公司 A kind of acoustical gypsum board and preparation method thereof
CN111876115A (en) * 2020-08-18 2020-11-03 上海澳昌实业有限公司 Organic silicon modified high-temperature-resistant epoxy structural adhesive and preparation method thereof
CN115820082A (en) * 2022-11-24 2023-03-21 国网浙江省电力有限公司超高压分公司 Thermosensitive color-changing temperature-indicating coating and preparation method thereof
CN115820082B (en) * 2022-11-24 2023-09-08 国网浙江省电力有限公司超高压分公司 Thermochromic temperature-indicating paint and preparation method thereof

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Application publication date: 20171103