CN108070168A - A kind of polyvinyl chloride-based high heat conductivity insulation composite and preparation method thereof - Google Patents
A kind of polyvinyl chloride-based high heat conductivity insulation composite and preparation method thereof Download PDFInfo
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- CN108070168A CN108070168A CN201611000260.4A CN201611000260A CN108070168A CN 108070168 A CN108070168 A CN 108070168A CN 201611000260 A CN201611000260 A CN 201611000260A CN 108070168 A CN108070168 A CN 108070168A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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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
- C08L27/00—Compositions of 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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of 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 a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2461/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2461/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/20—Applications use in electrical or conductive gadgets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2312/00—Crosslinking
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Abstract
The invention discloses a kind of polyvinyl chloride-based high heat conductivity insulation composites and preparation method thereof, are prepared including following parts by weight raw material：30 60 parts of polyvinyl chloride, 5 10 parts of hexamethylene dilute methanol, 10 25 parts of polyether-ether-ketone, 25 parts of cyclohexane-carboxylic acid, 25 parts of Nanometer sized lead oxide, 36 parts of carbon nano-fiber, 25 parts of nano-graphite, 13 parts of coupling agent, 15 parts of crosslinking agent；The present invention is made composite material have the advantages of heat conduction constant is big, high mechanical properties, is promoted application of the heat conductive insulating composite material on rapid cooling electronic device is needed using polymer crosslinking and organic inorganic hybridization principle.
Description
Technical field
The present invention relates to field of electronic materials, and in particular to a kind of polyvinyl chloride-based high heat conductivity insulation composite and its system
Preparation Method.
Background technology
The circuit design of electronic product becomes increasingly complex at present, in densification, trend toward miniaturization.These electronic and electrical equipments
Amount of heat can be generated, if these heats cannot discharge in time, accumulation to a certain extent will certainly be to the component of electronic apparatus
And equipment damages in itself.So the waste heat that must be generated is timely, is efficiently transferred in ambient enviroment.
Traditional metal material in heat dissipation industry, because the geometry of its product is very limited, and such radiator and electricity
Subcomponent surface is there are certain interval, so as to more and more easily be substituted by some thermal interfacial materials.
High molecular material electrical insulation capability is excellent, but thermal conductivity factor is very low, generally 0.2W/m.K, is only metal material
1 percent to one thousandth.Compare at present the application scenario that there should be high heat conduction for some while have insulating properties requirement again
More conventional method is inorganic filler (aluminium nitride, oxygen of the addition with high thermal conductivity coefficient and high impedance in polymer-based material
Change lead etc.), the patents such as CN02825187.3, CN200880011625.0 and CN201010194959.5 are all using this side
Method.But the material prepared in this way, since a large amount of additions of heat filling receive the mechanical property of composite material
Serious damage, while the raising of heat conductivility is not also notable, is generally hardly higher than 2W/m.K.For LED radiator, electric appliance
Radiator etc. needs the situation using radiator area flash heat transfer, if the thermal conductivity factor of material is small, in length direction
On heat transfer with regard to extremely difficult, heat, which is all concentrated in the region of very little, to spread, and the effective area of radiator is caused not have
It makes full use of, affects radiating efficiency.
The content of the invention
It is an object of the invention to overcome thermal conductivity factor existing for existing heat conductive insulating composite material low, poor mechanical property
Defect provides a kind of polyvinyl chloride-based high heat conductivity insulation composite and preparation method thereof；The present invention utilizes polymer crosslinking
With hybrid inorganic-organic principle, the advantages of thermal conductivity factor is big, and mechanical property is good is made it have, heat-conducting insulation material is promoted and exists
Need the application on the electronic device of rapid cooling.
In order to realize foregoing invention purpose, the present invention provides a kind of polyvinyl chloride-based high heat conductivity insulation composite, bags
Following parts by weight raw material are included to be prepared：30-60 parts of polyvinyl chloride, 5-10 parts of hexamethylene dilute methanol, 10-25 parts of polyethers
Ether ketone, 2-5 parts of cyclohexane-carboxylic acid, 2-5 parts of Nanometer sized lead oxide, 3-6 parts of carbon nano-fiber, 2-5 parts of nano-graphite, 1-
3 parts of coupling agent, 1-5 parts of crosslinking agent.
A kind of polyvinyl chloride-based high heat conductivity insulation composite using the polymerization that is cross-linked with each other of gas chromatography, forms knot
Structure is stablized, the polymer three-dimensional network structure of excellent in mechanical performance, while the hydridization difference Heat Conduction Material in three-dimensional net structure,
Lead oxide-carbon fiber-graphite three forms a three-dimensional heat radiating structure, and radiating rate increases, heat conductivility increase；Meanwhile three
Dimension network structure increases mechanical properties of polymer, operating temperature higher；The heat conductive insulating composite material use scope bigger,
Be conducive to the development of electronics industry.
Preferably, wherein the polyvinyl chloride polymerization degree is 200-500, the degree of polymerization is too big, and strand is too long, formation
It is poor that three-dimensional net structure is stablized, and composite material fusing point reduces；The degree of polymerization is too small, and strand is too short, is unfavorable for the miscellaneous of Heat Conduction Material
Change and embedded, Heat Conduction Material disperses irregularly, it is possible to create agglomeration, product heat conductivility reduce.
Preferably, wherein the polyether-ether-ketone degree of polymerization is 40-80, the degree of polymerization is too big, and strand is too long, and the three of formation
It ties up network structure and stablizes poor, composite materials property reduction；The degree of polymerization is too small, and strand is too short, is unfavorable for Heat Conduction Material
Hydridization and insertion, Heat Conduction Material disperse irregularly, it is possible to create agglomeration, product heat conductivility reduce.
Preferably, wherein the grain size of the Nanometer sized lead oxide is 20-60 nanometers, grain size is too big, is unfavorable for Heat Conduction Material
Hydridization in three-dimensional net structure and insertion, Heat Conduction Material disperse irregularly, it is possible to create agglomeration, product thermal conductivity
It can reduce, grain size is too small, difficulties in dispersion, easily reunites.
Preferably, wherein a diameter of 2-5nm of the carbon nano-fiber, length 10-50nm, diameter and length are too
Greatly, the hydridization in three-dimensional net structure and insertion, Heat Conduction Material for being unfavorable for Heat Conduction Material are disperseed irregularly, it is possible to create group
Poly- phenomenon, product heat conductivility reduce, and a diameter of 2-5nm, length is too small for 10-50nm, difficulties in dispersion, easily reunite, it is difficult to
The three-dimensional heat dissipation system of structure.
Preferably, wherein the grain size of the nano-graphite is 20-50 nanometers, grain size is too big, is unfavorable for Heat Conduction Material
Hydridization and insertion in three-dimensional net structure, Heat Conduction Material disperse irregularly, it is possible to create agglomeration, product heat conductivility
It reduces, grain size is too small, difficulties in dispersion, easily reunites.
Preferably, wherein the coupling agent is silane coupling agent, silane coupling agent to the coupling effect of Heat Conduction Material most
It is good.
Preferably, a kind of polyvinyl chloride-based high heat conductivity insulation composite is prepared including following parts by weight raw material
It forms：40-50 parts of polyvinyl chloride, 5-8 parts of hexamethylene dilute methanol, 15-20 parts of polyether-ether-ketone, 2-3 parts of cyclohexane-carboxylic acid,
2-3 parts of Nanometer sized lead oxide, 2-3 parts of carbon nano-fiber, 4-6 parts of nano-graphite, 1-2 parts of coupling agent, 2-3 parts of crosslinking
Agent.
In order to realize foregoing invention purpose, further, the present invention provides a kind of polyvinyl chloride-based high heat conductive insulatings to answer
The preparation method of condensation material, comprises the following steps：
（1）Nanometer sized lead oxide, carbon nano-fiber, nano-graphite are dispersed in hexamethylene dilute methanol and form suspension；
（2）The suspension that step 1 is obtained is esterified with cyclohexane-carboxylic acid, coupling agent, coupling reaction, obtains cyclohexane-carboxylic acid ring
Own dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and polyvinyl chloride that step 2 is obtained, polyether-ether-ketone, crosslinking
Cross-linking reaction is carried out after agent mixing, obtains polyvinyl chloride-based high heat conductivity insulation composite.
A kind of preparation method of polyvinyl chloride-based high heat conductivity insulation composite, first passes through hexamethylene dilute methanol by Heat Conduction Material
It is homodisperse to open, esterification and coupling agent is recycled to be coupled the ester of synthesis and Heat Conduction Material, forms cyclohexane-carboxylic acid hexamethylene
Dilute methanol ester hybridized mixed object so that the arrangement of the uniform rule of Heat Conduction Material is dispersed in three-dimensional net structure, will not reunite,
And lead oxide-carbon fiber-graphite three-dimensional radiator structure is formed, radiating rate increases, heat conductivility increase；Finally by with it is other
The crosslinking of high molecular material forms the polyvinyl chloride-based high heat conductivity insulation composite with three-dimensional net structure, makes polymerization
Object mechanical property increases, operating temperature higher；The preparation method of the polyvinyl chloride-based high heat conductivity insulation composite is simple, steady
It is fixed, reliable, it is suitble to extensive, the industrialized production of polyvinyl chloride-based high heat conductivity insulation composite.
Preferably, the esterification reaction temperature is 120-150 DEG C, and reaction temperature is excessively high, and reaction is violent, and control is difficult, instead
Answer temperature too low, reaction speed is slow, and the production cycle is long.
Preferably, the reaction time of esterification is 2-5h, and the reaction time is long, and the production cycle is long, and efficiency is low, the reaction time
Too short, reaction is incomplete, and product heat conductivility reduces.
Preferably, the cross-linking reaction temperature is 180-250 DEG C, and crosslinking temperature is excessively high, is crosslinked transition, the three dimensional network of formation
Network irregular structure, properties of product reduce, and crosslinking temperature is too low, and the reaction time is too long, and the production cycle is long.
Preferably, the time of the cross-linking reaction is 1-3h, and the reaction time is long, and the production cycle is long, and efficiency is low, during reaction
Between it is too short, reaction is incomplete, and product heat conductivility reduces.
Compared with prior art, beneficial effects of the present invention：
1st, the polyvinyl chloride-based high heat conductivity insulation composite of the present invention contains three-dimensional net structure and lead oxide-carbon fiber-graphite
Three-dimensional heat radiating structure has higher heat conductivility and mechanical property.
2nd, the preparation method of the polyvinyl chloride-based high heat conductivity insulation composite of the present invention first passes through esterification and hydridization, recycles
Crosslinking, by Heat Conduction Material Monodispersed in three-dimensional net structure system, parallel into lead oxide-carbon fiber-graphite three-dimensional heat dissipation knot
Structure, so as to add the radiating rate of composite material.
3rd, the preparation method of the polyvinyl chloride-based high heat conductivity insulation composite of the present invention is simple, stablizes, is reliable, is suitble to polychlorostyrene
Extensive, the industrialized production of vinyl high heat conductivity insulation composite.
Specific embodiment
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）The nano-graphite of the Nanometer sized lead oxide of 3 parts by weight, the carbon nano-fiber of 5 parts by weight, 4 parts by weight is dispersed in 10 weights
It measures in the hexamethylene dilute methanol of part and forms solution；
（2）Item of the solution and the cyclohexane-carboxylic acid of 3 parts by weight, the silane coupling agent of 2 parts by weight that step 1 is obtained at 120 DEG C
It is esterified under part, coupling reaction 5h, obtains cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and the degree of polymerization of 20 parts by weight that step 2 is obtained are 200
Polyvinyl chloride, the degree of polymerization of 5 parts by weight are 40 polyether-ether-ketone, after the crosslinking agent mixing of 2 parts by weight at a temperature of 180 DEG C into
Row cross-linking reaction 3h, obtains polyvinyl chloride-based high heat conductivity insulation composite.
Embodiment 2
（1）The nano-graphite of the Nanometer sized lead oxide of 2 parts by weight, the carbon nano-fiber of 3 parts by weight, 6 parts by weight is dispersed in 5 weight
Solution is formed in the hexamethylene dilute methanol of part；
（2）Solution and the cyclohexane-carboxylic acid of 2 parts by weight that step 1 is obtained, the coupling agent of 1 parts by weight are at a temperature of 150 DEG C
It is esterified, coupling reaction 2h, obtains cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and the degree of polymerization of 15 parts by weight that step 2 is obtained are 500
Polyvinyl chloride, the degree of polymerization of 10 parts by weight is 80 polyether-ether-ketone, after the crosslinking agent mixing of 3 parts by weight at a temperature of 250 DEG C
Cross-linking reaction 1h is carried out, obtains polyvinyl chloride-based high heat conductivity insulation composite.
Embodiment 3
（1）The nano-graphite of the Nanometer sized lead oxide of 2 parts by weight, the carbon nano-fiber of 3 parts by weight, 5 parts by weight is dispersed in 5 weight
Solution is formed in the hexamethylene dilute methanol of part；
（2）Solution and the cyclohexane-carboxylic acid of 5 parts by weight, the coupling agent of 1 parts by weight that step 1 is obtained are esterified, are coupled instead
Should, obtain cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and the polyvinyl chloride of 30 parts by weight that step 2 is obtained, 10 weights
The polyether-ether-ketone of part is measured, cross-linking reaction is carried out after the crosslinking agent mixing of 1 parts by weight, obtains polyvinyl chloride-based high heat conductive insulating composite wood
Material.
Embodiment 4
（1）The nano-graphite of the Nanometer sized lead oxide of 5 parts by weight, the carbon nano-fiber of 5 parts by weight, 3 parts by weight is dispersed in 15 weights
It measures in the hexamethylene dilute methanol of part and forms solution；
（2）Solution and the cyclohexane-carboxylic acid of 2 parts by weight, the coupling agent of 3 parts by weight that step 1 is obtained are esterified, are coupled instead
Should, obtain cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and the polyvinyl chloride of 60 parts by weight that step 2 is obtained, 5 weights
The polyether-ether-ketone of part is measured, cross-linking reaction is carried out after the crosslinking agent mixing of 1 parts by weight, obtains polyvinyl chloride-based high heat conductive insulating composite wood
Material.
Claims (10)
1. a kind of heat conductive insulating composite material, which is characterized in that be prepared including following parts by weight raw material：30-60 parts
Polyvinyl chloride, 5-10 parts of hexamethylene dilute methanol, 10-25 parts of polyether-ether-ketone, 2-5 parts of cyclohexane-carboxylic acid, 2-5 parts of nano oxygen
Change lead, 3-6 parts of carbon nano-fiber, 2-5 parts of nano-graphite, 1-3 parts of coupling agent, 1-5 parts of crosslinking agent.
2. heat conductive insulating composite material according to claim 1, which is characterized in that the polyvinyl chloride polymerization degree is 200-
500。
3. heat conductive insulating composite material according to claim 1, which is characterized in that the polyether-ether-ketone degree of polymerization is 40-
80。
4. heat conductive insulating composite material according to claim 1, which is characterized in that the grain size of the Nanometer sized lead oxide is
20-60nm。
5. heat conductive insulating composite material according to claim 1, which is characterized in that a diameter of 2- of the carbon nano-fiber
5nm, length 10-50nm.
6. heat conductive insulating composite material according to claim 1, which is characterized in that the grain size of the graphite is 20-50nm.
7. heat conductive insulating composite material according to claim 1, which is characterized in that prepared including following parts by weight raw material
It forms：40-50 parts of polyvinyl chloride, 5-8 parts of hexamethylene dilute methanol, 15-20 parts of polyether-ether-ketone, 2-3 parts of cyclohexane-carboxylic acid,
2-3 parts of Nanometer sized lead oxide, 2-3 parts of carbon nano-fiber, 4-6 parts of nano-graphite, 1-2 parts of coupling agent, 2-3 parts of crosslinking
Agent.
8. the preparation method of heat conductive insulating composite material described in a kind of claim 1, which is characterized in that comprise the following steps：
（1）Nanometer sized lead oxide, carbon nano-fiber, nano-graphite are dispersed in hexamethylene dilute methanol and form suspension；
（2）The suspension that step 1 is obtained is esterified with cyclohexane-carboxylic acid, coupling agent, coupling reaction, obtains cyclohexane-carboxylic acid ring
Own dilute methanol ester hybridized mixed object；
（3）The cyclohexane-carboxylic acid hexamethylene dilute methanol ester hybridized mixed object and polyvinyl chloride that step 2 is obtained, polyether-ether-ketone, crosslinking
Cross-linking reaction is carried out after agent mixing, obtains polyvinyl chloride-based high heat conductivity insulation composite.
9. preparation method according to claim 8, which is characterized in that esterification reaction temperature is 120-150 DEG C in step 2,
Time is 2-5h.
10. preparation method according to claim 8, which is characterized in that cross-linking reaction temperature is 180-250 DEG C in step 3,
Time is 1-3h.
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| CN201611000260.4A CN108070168A (en) | 2016-11-17 | 2016-11-17 | A kind of polyvinyl chloride-based high heat conductivity insulation composite and preparation method thereof |
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| CN201611000260.4A CN108070168A (en) | 2016-11-17 | 2016-11-17 | A kind of polyvinyl chloride-based high heat conductivity insulation composite and preparation method thereof |
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Application publication date: 20180525 |