CN106751477A - A kind of high-molecular-weight epoxy Heat Conduction Material and preparation method thereof - Google Patents
A kind of high-molecular-weight epoxy Heat Conduction Material and preparation method thereof Download PDFInfo
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- CN106751477A CN106751477A CN201611068176.6A CN201611068176A CN106751477A CN 106751477 A CN106751477 A CN 106751477A CN 201611068176 A CN201611068176 A CN 201611068176A CN 106751477 A CN106751477 A CN 106751477A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
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- 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
Abstract
The invention discloses a kind of high-molecular-weight epoxy Heat Conduction Material, it is made up of the raw material of following weight parts：Propenyl 23, TBAB 0.4 1, hexagonal boron nitride 37 40, methylhexahydrophthalic anhydride 8 10, acetylacetone,2,4-pentanedione neodymium 0.4 1, the diaminobenzoic acid 46 of octadecylamine 0.7 1,3,5, triphenyl phosphite 23, pyridine 0.3 0.5, N methyl pyrrolidones 32 40, epoxy resin E40100 110, polyacrylamide 0.6 1, sodium fluoborate 23, vinyl carboxylate 34, polybenzimidazoles 0.6 1, diatomite 10 12, lauryl glucosyl 0.3 1.The polyacrylamide that the present invention is added can effectively improve dispersiveness of the filler in interlaminar resin, improve the combination property of finished product.
Description
Technical field
The present invention relates to Heat Conduction Material technical field, more particularly to a kind of high-molecular-weight epoxy Heat Conduction Material and its preparation side
Method.
Background technology
Polymer Composites with High Thermal Conductivity as a kind of functional material of great application prospect, due to there is good heat
Conductive performance, thus played in many manufacturing industry such as microelectronics, Aeronautics and Astronautics, military equipment, electrical equipment and electrical and high-tech area
Very important effect.Particularly in recent years, with electronic integration technology high speed development, packing density is improved rapidly, electronics
Element, thousands of times of logic circuit volume ground reduces, electronic instrument and equipment is increasingly ultralight, thin, short, small direction is developed,
Under high-frequency work frequency, semiconductor operating thermal environment is moved rapidly to high temperature direction;Now, the heat that electronic component is produced is fast
Speed accumulation and increase, will make component remain to normally reliably run, and radiating in time turns into the key of restriction service life
Technology.Therefore with electronic component miniaturization, high performance, it is desirable to which material proposes requirements at the higher level to heat conductivility.At present
General polymeric material cannot meet the demand of development.Exploitation has Thermal conductivity, while having Jie higher again
The polymer matrix composite of electrical property and processability is for promoting microelectronics, Aero-Space, military equipment and motor electricity
The fields such as device fast development important in inhibiting；
Hexagonal boron nitride is a kind of III-V important race's chemicals, belongs to hexagonal crystal system, is most common in boron nitride there is shape
State, it has the similar layer structure with graphite, have the title of white graphite.Each layer of hexagonal AlN is former by B atoms and N
The hexagonal cyclic structure of the spaced plane of son, and B atoms and N atoms are one by SP2 hydridization Covalent bonding togethers
Rise, and combined by Van der Waals force between layers, therefore hexagonal AlN is stable per Rotating fields, but it is easy to stripping between layers
From.BN materials have many excellent performances, such as:High heat conduction, electric insulation, high temperature resistant, the anti-oxidant, coefficient of expansion are low, friction
Coefficient is low, chemical stability is good, processability is good, with good wave many advantages, such as, therefore be widely used in
The high-tech such as machinery, metallurgy, electronics, space flight and aviation is led the way.Over the years, the nano material such as BN nanotubes and nanometer sheet with
The discovery of CNT and Graphene also turns into the focus of current research.Technology of preparing to BN nanotubes is continued to develop, existing
Exploring the side such as arc discharge method, laser ablation method, mechanical attrition method, CNT template, chemical vapour deposition technique
Method can successfully prepare BN nanotubes, and do substantial amounts of research to its function dough and application；
Epoxy resin has excellent mechanical property, electrical property, adhesive property and thermally-stabilised, be widely used to Aero-Space,
The field such as electric.Epoxy resin is various in style, and what this work was selected is cycloaliphatic epoxy resin, due to aliphatic ring oxygen tree
Epoxide group in fat molecular structure is not from expoxy propane, and epoxy radicals is connected directly between on alicyclic ring, so alicyclic epoxy
Resin compared with bisphenol-A type epoxy resin, with good heat endurance, excellent electrical insulation capability and weather resisteant, height
Security many advantages, such as.It is difficult but the thermal conductivity factor of epoxy resin is relatively low (0.23 W/m K), and heat dispersion is poor
To meet the fast development of microelectric technique and encapsulation technology；
The thermal conductivity factor of polymer matrix composite is not only relevant with the thermal conductivity factor that it constitutes each phase, but also with each component
Relative amount, form, distribution and interaction are relevant.Filler grain content, shape of particle, distribution etc. can all be led to system
Hot coefficient is produced a very large impact.At present, many researchers are according to minimum thermal resistance method, Thermal self-ignition and homogenize method scheduling theory,
The model of many prediction binary system thermal conductivities is set up, big multi-model is suitable only for corresponding system, and universality is not high.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of high-molecular-weight epoxy Heat Conduction Material and its system
Preparation Method.
The present invention is achieved by the following technical solutions：
A kind of high-molecular-weight epoxy Heat Conduction Material, it is made up of the raw material of following weight parts：
Propenyl 2-3, TBAB 0.4-1, hexagonal boron nitride 37-40, methylhexahydrophthalic anhydride 8-10, acetyl
Acetone neodymium 0.4-1, octadecylamine 0.7-1,3,5- diaminobenzoic acids 4-6, triphenyl phosphite 2-3, pyridine 0.3-0.5, N- first
Base pyrrolidones 32-40, epoxy resin E40100-110, polyacrylamide 0.6-1, sodium fluoborate 2-3, vinyl carboxylate 3-
4th, polybenzimidazoles 0.6-1, diatomite 10-12, lauryl glucosyl 0.3-1.
A kind of preparation method of described high-molecular-weight epoxy Heat Conduction Material, comprises the following steps：
（1）Above-mentioned TBAB, diatomite are mixed, is added in the deionized water of 10-15 times of compound weight, stirred
Uniformly, the sulfuric acid solution of 4-6mol/l is added dropwise, regulation pH is 2-3, it is 70-75 DEG C, insulated and stirred 1-2 hours, mistake to rise high-temperature
Filter, by precipitation washing 3-4 times, air drying obtains modification infusorial earth；
（2）Above-mentioned hexagonal boron nitride is added in the DMF of 35-40 times of its weight, ultrasonic 100-120 points
Clock, is centrifuged in the centrifuge of 5000-8000rpm, collects upper solution, suction filtration, by filter cake as in vacuum drying oven, 60-70
Dried completely at DEG C, obtain stripping boron nitride；
（3）By above-mentioned stripping boron nitride, modification infusorial earth, octadecylamine mix, as 190-200 DEG C of oil bath in, be passed through nitrogen,
Insulated and stirred 90-100 hours, discharging was cooled to room temperature, added the tetrahydrofuran of 10-12 times of compound weight, stirring reaction
100-130 minutes, precipitation methyl alcohol was washed in filtering 3-4 times, is placed in 110-120 DEG C of vacuum drying oven and is dried 100-150 points
Clock, obtains octadecylamine grafting boron nitride；
（4）Above-mentioned polybenzimidazoles is added in the DMA of 17-20 times of its weight, is stirred, raised
Temperature is 76-80 DEG C, insulated and stirred 5-7 minutes, obtains acid amides dispersion liquid；
（5）Above-mentioned octadecylamine grafting boron nitride is added in 1-METHYLPYRROLIDONE, is stirred, add above-mentioned 3,5- diaminos
Yl benzoic acid, triphenyl phosphite, pyridine, are passed through nitrogen, are reacted 3-4 hours at 100-110 DEG C, discharging cooling, are added to
Mass ratio be 0.1% lithium chloride methanol solvate in carry out precipitating, be separated by filtration, precipitation is added to above-mentioned acid amides dispersion liquid
In, stirring, suction filtration washes filter cake absolute ethyl alcohol 2-3 times, is vacuum dried 2-3 hours at 90-100 DEG C, obtains hyperbranched
Modified boron nitride；
（6）Above-mentioned sodium fluoborate, hyperbranched modified boron nitride are mixed, the deionized water of 17-20 times of compound weight is added to
In, stir, above-mentioned polyacrylamide is added, insulated and stirred 1-2 hours at 60-70 DEG C, filtering, by precipitation washing 2-3
Secondary, air drying obtains compound hyperbranched modified boron nitride；
（7）Above-mentioned acetylacetone,2,4-pentanedione neodymium, epoxy resin E40 are mixed, is stirred 1-2 hours at 80-90 DEG C, be added to compound weight
In the acetone of 7-10 times of amount, stir, add above-mentioned compound hyperbranched modified boron nitride, it is ultrasonic 20-30 minutes, as 70-
It is in 75 DEG C of oil bath, acetone solvent volatilization is clean, remaining each raw material is added, stir, it is placed in steel mold, first in 135-
Precuring 100-110 minutes at 140 DEG C, temperature is then raised to 165-170 DEG C, solidified 10-15 hours, cooling is obtained final product.
It is an advantage of the invention that：
The present invention can be efficiently peeled off hexagonal AlN powder using the method for ultrasound centrifugation first, because inside BN,
Hexatomic ring in each layer is relatively independent, the phenomenon not misplaced between them, and is considered as on vertical direction
Parallel, meanwhile, be combined in the form of very strong covalent bond between the atom in layer, thus compact conformation, but each layer it
Between be then combined in the form of weaker Van der Waals force, due to its layer of BN powder and layer relatively weak adhesion and distance
It is larger, so each interlayer of BN powder is relatively easily slided and peeled off in the presence of ultrasonic wave；Then repaiied using octadecylamine molecule
The BN nanometer sheets peeled off are adornd, because the end group amino in octadecylamine is that electron rich serves as Lewis acid, and in BN nanometer sheets
B atoms are that electron deficient serves as Lewis alkali, can by the interaction octadecylamine molecule of the non-covalent bond of Lewis soda acids
To be particularly well adsorbed in BN nanometer sheets surface, it is modified after BN nanometer sheets surface octadecylamine long-chain molecule in asphalt mixtures modified by epoxy resin
Molecular entanglement can occur with epoxy molecule in fat solidification process and produce a good interface interaction, form many physics and hand over
Connection point, enhances its heat conductivility, is finally distributed in epoxy resin-base by hyperbranched being modified again, and with good point
Property and compatibility are dissipated, because the end group of the Hyperbranched Aromatic Polyamides of hyperbranched modified nitridation boron surface has substantial amounts of amino group,
Epoxide group with epoxy resin can chemically react, and enhance the interaction between modified boron nitride and epoxy resin interface
Power, this action effect increased the chemical crosslinking point in epoxy resin cure network, crosslinking points in epoxy resin three-dimensional network
The heat conductivility for increasing the interface resistance that can be reduced between modified boron nitride and epoxy resin, substantially increasing composite.
The polyacrylamide that the present invention is added can effectively improve dispersiveness of the filler in interlaminar resin, improve the combination property of finished product.
Specific embodiment
A kind of high-molecular-weight epoxy Heat Conduction Material, it is made up of the raw material of following weight parts：
Propenyl 2, TBAB 0.4, hexagonal boron nitride 37, methylhexahydrophthalic anhydride 8, acetylacetone,2,4-pentanedione neodymium 0.4,
The diaminobenzoic acid 4 of octadecylamine 0.7,3,5, triphenyl phosphite 2, pyridine 0.3,1-METHYLPYRROLIDONE 32, epoxy resin E40
100th, polyacrylamide 0.6, sodium fluoborate 2, vinyl carboxylate 3, polybenzimidazoles 0.6, diatomite 10, dodecyl grape
Glucosides 0.3.
A kind of preparation method of described high-molecular-weight epoxy Heat Conduction Material, comprises the following steps：
（1）Above-mentioned TBAB, diatomite are mixed, is added in the deionized water of 10 times of compound weight, stirring is equal
It is even, the sulfuric acid solution of 4mol/l is added dropwise, regulation pH is 2, and it is 70 DEG C to rise high-temperature, and insulated and stirred 1 hour, filtering will precipitate water
Wash 3 times, air drying obtains modification infusorial earth；
（2）Above-mentioned hexagonal boron nitride is added in the DMF of 35 times of its weight, ultrasound 100 minutes,
Be centrifuged in the centrifuge of 5000rpm, collect upper solution, suction filtration, by filter cake as vacuum drying oven in, dried at 60 DEG C it is complete,
Boron nitride must be peeled off；
（3）By above-mentioned stripping boron nitride, modification infusorial earth, octadecylamine mix, as 190 DEG C of oil baths in, be passed through nitrogen, be incubated
Stirring 90 hours, discharging is cooled to room temperature, adds the tetrahydrofuran of 10 times of compound weight, and stirring reaction 100 minutes is filtered,
Precipitation methyl alcohol is washed 3 times, is placed in 110 DEG C of vacuum drying oven and is dried 100 minutes, obtain octadecylamine grafting boron nitride；
（4）Above-mentioned polybenzimidazoles is added to the N of 17 times of its weight, in N dimethyl acetamide, is stirred, rise high-temperature
It it is 76 DEG C, insulated and stirred 5 minutes obtains acid amides dispersion liquid；
（5）Above-mentioned octadecylamine grafting boron nitride is added in N methyl pyrrolidones, is stirred, add above-mentioned 3,5 diaminourea
Benzoic acid, triphenyl phosphite, pyridine, are passed through nitrogen, are reacted 3 hours at 100 DEG C, discharging cooling, and being added to mass ratio is
Precipitating is carried out in the methanol solvate of 0.1% lithium chloride, is separated by filtration, precipitation is added in above-mentioned acid amides dispersion liquid, stirring is equal
Even, suction filtration washes filter cake absolute ethyl alcohol 2 times, is vacuum dried 2 hours at 90 DEG C, obtains hyperbranched modified boron nitride；
（6）Above-mentioned sodium fluoborate, hyperbranched modified boron nitride are mixed, are added in the deionized water of 17 times of compound weight,
Stir, add above-mentioned polyacrylamide, precipitation is washed in insulated and stirred 1 hour at 60 DEG C, filtering 2 times, and normal temperature is done
It is dry, obtain compound hyperbranched modified boron nitride；
（7）Above-mentioned acetylacetone,2,4-pentanedione neodymium, epoxy resin E40 are mixed, is stirred 1 hour at 80 DEG C, be added to 7 times of compound weight
Acetone in, stir, add it is above-mentioned be combined hyperbranched modified boron nitride, ultrasound 20 minutes, as in 70 DEG C of oil baths, will
Acetone solvent volatilization is clean, adds remaining each raw material, stirs, and is placed in steel mold, first 100 points of precuring at 135 DEG C
Clock, is then raised to 165 DEG C by temperature, solidifies 10 hours, and cooling is obtained final product.
Performance test：
Its thermal conductivity factor is 0.57 W/mK at 25 DEG C.
Claims (2)
1. a kind of high-molecular-weight epoxy Heat Conduction Material, it is characterised in that it is made up of the raw material of following weight parts：
Propenyl 2-3, TBAB 0.4-1, hexagonal boron nitride 37-40, methylhexahydrophthalic anhydride 8-10, acetyl
Acetone neodymium 0.4-1, octadecylamine 0.7-1,3,5- diaminobenzoic acids 4-6, triphenyl phosphite 2-3, pyridine 0.3-0.5, N- first
Base pyrrolidones 32-40, epoxy resin E40100-110, polyacrylamide 0.6-1, sodium fluoborate 2-3, vinyl carboxylate 3-
4th, polybenzimidazoles 0.6-1, diatomite 10-12, lauryl glucosyl 0.3-1.
2. a kind of preparation method of high-molecular-weight epoxy Heat Conduction Material as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Above-mentioned TBAB, diatomite are mixed, is added in the deionized water of 10-15 times of compound weight, stirred
Uniformly, the sulfuric acid solution of 4-6mol/l is added dropwise, regulation pH is 2-3, it is 70-75 DEG C, insulated and stirred 1-2 hours, mistake to rise high-temperature
Filter, by precipitation washing 3-4 times, air drying obtains modification infusorial earth；
（2）Above-mentioned hexagonal boron nitride is added in the DMF of 35-40 times of its weight, ultrasonic 100-120 points
Clock, is centrifuged in the centrifuge of 5000-8000rpm, collects upper solution, suction filtration, by filter cake as in vacuum drying oven, 60-70
Dried completely at DEG C, obtain stripping boron nitride；
（3）By above-mentioned stripping boron nitride, modification infusorial earth, octadecylamine mix, as 190-200 DEG C of oil bath in, be passed through nitrogen,
Insulated and stirred 90-100 hours, discharging was cooled to room temperature, added the tetrahydrofuran of 10-12 times of compound weight, stirring reaction
100-130 minutes, precipitation methyl alcohol was washed in filtering 3-4 times, is placed in 110-120 DEG C of vacuum drying oven and is dried 100-150 points
Clock, obtains octadecylamine grafting boron nitride；
（4）Above-mentioned polybenzimidazoles is added in the DMA of 17-20 times of its weight, is stirred, raised
Temperature is 76-80 DEG C, insulated and stirred 5-7 minutes, obtains acid amides dispersion liquid；
（5）Above-mentioned octadecylamine grafting boron nitride is added in 1-METHYLPYRROLIDONE, is stirred, add above-mentioned 3,5- diaminos
Yl benzoic acid, triphenyl phosphite, pyridine, are passed through nitrogen, are reacted 3-4 hours at 100-110 DEG C, discharging cooling, are added to
Mass ratio be 0.1% lithium chloride methanol solvate in carry out precipitating, be separated by filtration, precipitation is added to above-mentioned acid amides dispersion liquid
In, stirring, suction filtration washes filter cake absolute ethyl alcohol 2-3 times, is vacuum dried 2-3 hours at 90-100 DEG C, obtains hyperbranched
Modified boron nitride；
（6）Above-mentioned sodium fluoborate, hyperbranched modified boron nitride are mixed, the deionized water of 17-20 times of compound weight is added to
In, stir, above-mentioned polyacrylamide is added, insulated and stirred 1-2 hours at 60-70 DEG C, filtering, by precipitation washing 2-3
Secondary, air drying obtains compound hyperbranched modified boron nitride；
（7）Above-mentioned acetylacetone,2,4-pentanedione neodymium, epoxy resin E40 are mixed, is stirred 1-2 hours at 80-90 DEG C, be added to compound weight
In the acetone of 7-10 times of amount, stir, add above-mentioned compound hyperbranched modified boron nitride, it is ultrasonic 20-30 minutes, as 70-
It is in 75 DEG C of oil bath, acetone solvent volatilization is clean, remaining each raw material is added, stir, it is placed in steel mold, first in 135-
Precuring 100-110 minutes at 140 DEG C, temperature is then raised to 165-170 DEG C, solidified 10-15 hours, cooling is obtained final product.
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| CN116759706A (en) * | 2023-07-17 | 2023-09-15 | 广东中宇恒通电热科技有限公司 | High-temperature-resistant high-humidity safe heating film |
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