CN104045896B - Heat conduction composite polyethylene material and preparation method thereof - Google Patents
Heat conduction composite polyethylene material and preparation method thereof Download PDFInfo
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- CN104045896B CN104045896B CN201410253603.2A CN201410253603A CN104045896B CN 104045896 B CN104045896 B CN 104045896B CN 201410253603 A CN201410253603 A CN 201410253603A CN 104045896 B CN104045896 B CN 104045896B
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention provides a kind of heat conduction composite polyethylene material and preparation method thereof.This heat conduction composite polyethylene material includes the polyethylene of 15～50 parts, the heat conducting fiber of 4～35 parts and the heat conduction particle of 23～80 parts by weight.In this heat conduction composite polyethylene material, by heat conducting fiber being added to base polyethylene as heat filling, define heat conduction composite polyethylene material.For granular heat filling, in fibrous heat conducting fiber after entering base polyethylene, being more readily formed overlap joint state each other, the lapping network formed is also easier to run through whole base polyethylene.Under the conduction of heat of such lapping network, the heat in matrix quickly spreads, thus is conducive to improving the heat transfer efficiency of composite.After being simultaneously introduced heat conduction particle, these heat conduction particles " can wrap up " joint between different heat conducting fiber, makes to form higher thermal conducting path between heat conducting fiber.
Description
Technical field
The present invention relates to polymeric material manufacture field, in particular to a kind of heat conduction composite polyethylene material and
Preparation method.
Background technology
Along with the development of science and technology, electronic applications and LED field are to the requirement of the power of device and integrated level day by day
Improving, correspondingly, high power and high integration make device heat amount in normal operation more and more higher.This just requires
Device has higher heat transfer property, to reach radiating effect timely.As the important material of preparing of these devices, polymer
The heat conductivility of material also receives increasing challenge.The polymerization that current most thermal conductive polymer composite uses
Thing matrix is polyphenylene sulfide and polyamide.But, these materials or processing characteristics are poor, or price is higher, should not advise greatly
Prepared by the production of mould.
Polyethylene is typical thermoplastic, and its body odorless, tasteless, nontoxic, material is soft and tough, density is lower than water,
And there are the dielectric properties of excellence.Meanwhile, the chemical stability of polyethylene is preferable, can be with resistance to most soda acid salt, room temperature
Down insoluble in any organic solvent.It addition, the resistance to low temperature of polyethylene is excellent, at-60 DEG C, it still is able to keep good power
Learn performance.As a kind of engineering plastics, the temperature flowing of polyethylene is good, and processing characteristics is excellent, and it is excellent to have obvious cost
Gesture.Summary reason, the thermal conductive polymer composite with polyethylene as polymeric matrix becomes new study hotspot.
Patent CN102311568B discloses the preparation method of a kind of heat conduction high-density polyethylene material, and cardinal principle is to adopt
With the granular heat filling filling high-density polyethylene such as carborundum, aluminium nitride, to prepare heat conduction high-density polyethylene material.
The thermal conductivity of above-mentioned material is relatively low, and its high heat conductance only has 0.69w/ (mk).
Patent CN102311567B discloses the polyethylene Heat Conduction Material that a kind of nano aluminium oxide is filled, but its thermal conductivity is also
Relatively low.When nano aluminium oxide loading reaches 59%, the thermal conductivity of material only has 0.616w/ (mk).
In sum, the thermal conductivity how improving composite polyethylene material becomes the new focus of attention of researcher.
Summary of the invention
It is desirable to provide a kind of heat conduction composite polyethylene material and preparation method thereof, to solve poly-second in prior art
The problem that the heat conductivility of alkene composite is relatively low.
To achieve these goals, according to an aspect of the invention, it is provided a kind of heat conduction composite polyethylene material, its
Include the polyethylene of 15～50 parts, the heat conducting fiber of 4～35 parts and the heat conduction particle of 23～80 parts by weight.
Further, by weight, heat conducting fiber includes the long fibre of 2～20 parts and the chopped fiber of 2～15 parts；Long fibre
A length of the 0.7～9mm of dimension, a length of the 0.15 of chopped fiber～0.4mm.
Further, the thermal conductivity of above-mentioned heat conducting fiber > 80w/ (mk), the hot strength of heat conducting fiber > 700Mpa.
Further, by weight, heat conduction particle includes the expanded graphite of 20～50 parts and the scale stone of 3～30 parts
Ink.
Further, the initial expansion temperature of expanded graphite is 250～280 DEG C；The particle diameter of expanded graphite is 100～300
Mesh, the particle diameter of crystalline flake graphite is 1200～5000 mesh.
Further, heat conducting fiber is carbon fiber or metallic fiber, preferably carbon fiber.
Further, by weight, also include that the reinforcing fiber of 1～15 part, preferably reinforcing fiber are glass fibre.
Further, by weight, heat conduction composite polyethylene material also includes: the fire retardant of 1～20 part and 0.5～6
Fire retarding synergist, the toughener of optional 3～15 parts and the coupling agent of optional 0.5～3 part, preferably fire retardant of part are ten
One or more in dibromodiphenyl ether, TDE or tetrabromobisphenol A；Preferably fire retarding synergist is antimony oxide, antimony
One or more in acid sodium or Firebrake ZB；Preferably toughener be ethylene-vinyl acetate copolymer, ethylene propylene diene rubber, ethylene-
One or more in octene copolymer, SB；Preferably coupling agent is silane coupler.
According to a further aspect in the invention, additionally providing the preparation method of a kind of heat conduction composite polyethylene material, it includes
Following steps: S1, by weight, by the polyethylene of 15～50 parts, the heat conducting fiber of 4～35 parts, and 23～80 parts lead
Hot granule mixes in mixer, obtains mixture；S2, carry out mixture extruding, drawing and pelletize, obtain heat conduction and gather
Ethylene composite.
Further, in step S1, also include adding in mixer by the reinforcing fiber of 1～15 part by weight,
The step mixed jointly is carried out with polyethylene, heat conducting fiber and heat conduction particle.
Further, in step S1, also include the fire-retardant association of the fire retardant by by weight 1～20 part and 0.5～6 part
Effect agent adds in mixer, jointly carries out the step mixed with polyethylene, heat conducting fiber, heat conduction particle and optional reinforcing fiber
Suddenly.
Further, in step S1, before polyethylene is added in mixer, toughness reinforcing by polyethylene and 3～15 parts
Agent mix, and by mixture at a temperature of-60～-20 DEG C pulverizing to particle diameter below 150 μm.
Further, in step S1, heat conduction particle includes the expanded graphite of 20～50 parts and the crystalline flake graphite of 3～30 parts；
Before being added in mixer by crystalline flake graphite, also include the step that crystalline flake graphite is carried out pretreatment；Crystalline flake graphite is carried out
The step of pretreatment includes: by weight, is dissolved in ethanol by the coupling agent of 0.3～2 part, and being configured to concentration is 1～3%wt
The first mixed solution, the first mixed solution is sprayed in crystalline flake graphite, and mixes in mixer, take out dried formation
The crystalline flake graphite of pretreatment.
Further, in step S1, before reinforcing fiber being added in mixer, also include carrying out pre-to reinforcing fiber
The step processed；The step that reinforcing fiber carries out pretreatment includes: by weight, and the coupling agent of 0.2～1 part is dissolved in second
In alcohol, it is configured to the second mixed solution that concentration is 1～3%wt, the second mixed solution is sprayed to reinforcing fiber, drying
After, form the reinforcing fiber of pretreatment.
Further, in step S2, when being extruded by mixture, extrusion temperature is 200～270 DEG C.
Heat conduction composite polyethylene material and preparation method thereof of the application present invention, by using heat conducting fiber as heat filling
Add to base polyethylene, define heat conduction composite polyethylene material.For granular heat filling, in fiber
The heat filling of shape, after entering base polyethylene, is more readily formed overlap joint state each other, and the lapping network formed is also
It is easier to run through whole base polyethylene.Under the conduction of heat of such lapping network, it is possible to promote the heat in matrix
Quickly diffusion, thus be conducive to improving the heat transfer efficiency of composite, and then improve the radiating effect of composite.It addition,
When composite is by external impacts, the lapping network that fibrous heat filling is formed can also utilize the deformation of self to inhale
Receive certain energy, thus improve the shock resistance of composite, make composite have higher mechanical property.Add simultaneously
After entering heat conduction particle, these heat conduction particles " can wrap up " joint between different heat conducting fiber, makes to be formed between heat conducting fiber
Higher thermal conducting path.The most such as, heat conduction particle " can also pierce " position between heat conducting fiber, promotes originally to be located remotely from each other
Heat conducting fiber by these heat conduction particles formed thermal conducting path.Under effect in every respect, be conducive to making two kinds of heat fillings
Mutually coordinated, base polyethylene is formed more perfect three-dimensional net structure.Thus improve the heat conduction of composite further
Performance, and improve the shock resistance of composite.
Detailed description of the invention
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can phases
Combination mutually.The present invention is described in detail below in conjunction with embodiment.
As background section is introduced, existing composite polyethylene material has the problem that heat conductivity is poor.For
Solving this problem, inventor provides a kind of heat conduction composite polyethylene material, by weight, it include 15～
The polyethylene of 50 parts and the heat conducting fiber of 4～35 parts and the heat conduction particle of 23～80 parts.
The above-mentioned composite of the present invention, is heat conducting fiber and heat conduction particle to be added to poly-second simultaneously as heat filling
In thiazolinyl body.For granular heat filling, in fibrous heat filling after entering base polyethylene, mutually
Between be more readily formed overlap joint state, the lapping network formed is also easier to run through whole base polyethylene.Take such
Connect under the conduction of heat of network, it is possible to promote the heat in matrix quickly to spread, thus be conducive to improving the biography of composite
The thermal efficiency, and then improve the radiating effect of composite.It addition, when composite is by external impacts, fibrous heat conduction
The lapping network that filler is formed can also utilize the deformation of self to absorb certain energy, thus improves the anti-impact of composite
Hit performance, make composite have higher mechanical property.After being simultaneously introduced heat conduction particle, these heat conduction particles can " wrap up "
Joint between different heat conducting fiber, makes to form higher thermal conducting path between heat conducting fiber.The most such as, heat conduction particle can also
" pierce " position between heat conducting fiber, promote the heat conducting fiber being originally located remotely from each other to form heat conduction by these heat conduction particles and lead to
Road.Under effect in every respect, be conducive to making two kinds of heat fillings mutually coordinated, base polyethylene is formed more perfect three
Dimension network structure.Thus improve the heat conductivility of composite further, and improve the shock resistance of composite.
In the above-mentioned composite of the present invention, as long as using heat conducting fiber as heat filling, it becomes possible at polyvinyl
The heat conduction network that in body, performance is certain.In a preferred embodiment, above-mentioned heat conducting fiber includes the long fibre of 2～20 parts
With the chopped fiber of 2～15 parts；Long stapled a length of 0.7～9mm, a length of the 0.15 of chopped fiber～0.4mm.In fixing heat conduction
In the case of filler number, heat conducting fiber collocation different for length is used, utilizes long fibre to form the filler on two-dimensional directional
Network, utilizes the two-dimentional filler network that chopped fiber overlap joint is different, and then can form three-dimensional filler network.This is advantageous for into one
Step improves heat conductivility and the shock resistance of composite.
In the above-mentioned composite of the present invention, the thermal conductivity of the heat conducting fiber used self is the highest, applies prepared by it
The heat conductivility of composite polyethylene material more preferable.Consider heat conductivility and the serviceability of composite, it is preferable that lead
The thermal conductivity of thermal fiber > 80w/ (mk), the hot strength of heat conducting fiber > 700Mpa.
In the above-mentioned composite of the present invention, the heat conduction particle of employing can be well-known to those skilled in the art arbitrarily
Carborundum that heat conduction particle, such as background section are previously mentioned and aluminium nitride.In a preferred embodiment, by weight
Part meter, above-mentioned heat conduction particle includes the expanded graphite of 20～50 parts and the crystalline flake graphite of 3～30 parts.Expanded graphite and crystalline flake graphite
It is respectively provided with higher heat conductivity, and the density of the two is lighter, it is possible to make composite have higher heat transfer property and lighter concurrently
Weight.It is highly preferred that the initial expansion temperature of above-mentioned expanded graphite is 250～280 DEG C；The particle diameter of expanded graphite be 100～
300 mesh, the particle diameter of crystalline flake graphite is 1200～5000 mesh.Initial expansion temperature be affect expanded graphite interlamellar spacing important because of
Element.The expanded graphite formed under above-mentioned initial expansion temperature, interlamellar spacing is the most suitable, it is possible to make the squama under the above-mentioned particle diameter of part
Sheet graphite enters interlayer.It is thus possible to improve the heat conductivility of expanded graphite further, to improve leading of composite further
Hot property.
In the above-mentioned composite of the present invention, the fiber arbitrarily with heat conductivility all potentially acts as above-mentioned heat conducting fiber.
In a preferred embodiment, above-mentioned heat conducting fiber is carbon fiber or metallic fiber, and metallic fiber can be copper fiber, aluminum
Fiber etc..It is highly preferred that above-mentioned heat conducting fiber is carbon fiber.Carbon fiber has higher thermal conductivity, and has high intensity, light weight
Advantage.In order to be conducive to the excellence making composite have high heat conduction, high impact resistance and high intensity concurrently as heat conducting fiber
Performance.In addition, for the consideration of raising Compound Material Engineering intensity further, above-mentioned composite by weight, is gone back
Including the reinforcing fiber of 1～15 part, this reinforcing fiber can be glass fibre.
According to the teaching that the present invention is above-mentioned, those skilled in the art, for improving the purpose of composite material combination property, have
Ability selects other auxiliary agents, is added in above-mentioned composite.One preferred embodiment in, by weight, above-mentioned
Composite also includes the fire retardant of 1～20 part and the fire retarding synergist of 0.5～6 part.Fire retardant and fire retarding synergist are added
In composite, it is possible to improve the fire resistance of composite, so that this composite is more suitable for the electronics device of high integration
Part prepare material.Concrete fire retardant includes but not limited in deca-BDE, TDE or tetrabromobisphenol A
Planting or multiple, fire retarding synergist includes but not limited to one or more in antimony oxide, sodium antimonate or Firebrake ZB；
It is highly preferred that by weight, above-mentioned heat conduction composite polyethylene material of stating also includes the toughener of 3～15%；Increase
Tough dose includes but not limited to ethylene-vinyl acetate copolymer, ethylene propylene diene rubber, ethylene-octene copolymer, styrene-fourth two
One or more in alkene copolymer；
It is further preferred that by weight, above-mentioned heat conduction composite polyethylene material also includes the coupling agent of 0.5～3 part；
Coupling agent includes but not limited to silane coupler.Utilize coupling agent, be conducive to improving between filler or auxiliary agent and base polyethylene
The compatibility, thus improve the combination property of composite further.
In the above-mentioned composite of the present invention, the molecular weight of the base polyethylene of employing does not has particular/special requirement, if its tool
There is preferable processing characteristics.Such as, the weight average molecular weight of polyethylene can be with 4 × 105～8 × 105。
It addition, present invention also offers the preparation method of a kind of heat conduction composite polyethylene material, it comprises the following steps:
S1, by weight, by the heat conduction particle of the polyethylene of 15～50 parts, the heat conducting fiber of 4～35 parts and 23～80 parts in mixing
Machine mixes, obtains mixture；S2, carry out described mixture extruding, drawing and pelletize, obtain described heat conduction polyethylene
Composite.Apply fibrous heat filling, it is possible to make to be formed between different heat conducting fiber lapping network, and then formation is led
Ther mal network.Even if the heat in matrix just can be transferred out by this by this heat conduction network, thus be conducive to improving poly-second
The heat conductivility of alkene composite.Meanwhile, when composite is by external force, such lapping network can utilize the shape of self
Become and absorb portion of energy, thus be conducive to improving the shock resistance of composite.Additionally, be simultaneously introduced threadiness and graininess
Heat filling, be conducive in base polyethylene, form more perfect three dimentional heat conduction filler network, thus improve multiple further
The heat conductivility of condensation material.
It is highly preferred that in above-mentioned steps S1, also include the reinforcing fiber of 1～15 part by weight is added mixer
In, the step mixed jointly is carried out with polyethylene, heat conducting fiber and heat conduction particle.By adding reinforcing fiber, it is possible to further
Improve the mechanical property of composite.It is further preferred that in above-mentioned steps S1, also include by weight 1～20 part
The fire retarding synergist of fire retardant and 0.5～6 part adds in mixer, with polyethylene, heat conducting fiber, heat conduction particle and optionally increase
Strong fiber carries out the step mixed jointly.By adding fire retardant and fire retarding synergist, it is possible to improve the anti-flammability of composite
Energy.
In the above-mentioned preparation method of the present invention, as long as each raw material is mixed in mixer, then mixture is squeezed
Go out, just can obtain the composite that heat conductivility is higher.One preferred embodiment in, in above-mentioned steps S1, will be poly-
Before ethylene adds in mixer, by polyethylene and the toughener mixing of 3～15 parts by weight, and by mixture-60
～at a temperature of-20 DEG C pulverizing to particle diameter below 150 μm.Polyethylene is ground at low temperatures in flour mill, it is possible to make it have
There is a less particle diameter, thus the beneficially mixing in later stage and extrusion processing.Meanwhile, add toughener further, be conducive to into one
Step improves the shock resistance of composite.
Above-mentioned heat conduction particle can be expanded graphite and crystalline flake graphite, it is preferable that in above-mentioned steps S1, heat conduction particle includes
The expanded graphite of 20～50 parts and the crystalline flake graphite of 3～30 parts；Before crystalline flake graphite is added in mixer, also include squama
Sheet graphite carries out the step of pretreatment；The step that crystalline flake graphite carries out pretreatment includes: by weight, by 0.3～2 part
Coupling agent is dissolved in ethanol, is configured to the first mixed solution that concentration is 1～3%wt, sprays the first mixed solution to scale
In graphite, and mix in mixer, take out the crystalline flake graphite forming pretreatment after drying.Utilize coupling agent to crystalline flake graphite
Carry out pretreatment, it is possible to improve the surface activity of crystalline flake graphite so that it is with base polyethylene, there is the more preferable compatibility, Jin Erti
The combination property of high composite.In like manner, in above-mentioned steps S1, before reinforcing fiber being added in mixer, it is right also to include
Reinforcing fiber carries out the step of pretreatment；The step that reinforcing fiber carries out pretreatment includes: by weight, by 0.2～1 part
Coupling agent be dissolved in ethanol, be configured to the second mixed solution that concentration is 1～3%wt, by second mixed solution spray to institute
State in reinforcing fiber, after drying, form the described reinforcing fiber of pretreatment.
In the above-mentioned preparation method of the present invention, when extruding polyethylene, filler mixture, expressing technique is according to routine
Polyethylene expressing technique.In a preferred embodiment, in above-mentioned steps S2, when mixture is extruded,
Extrusion temperature is 200～270 DEG C.The composite polyethylene material formed at such a temperature, heat conducting fiber, heat conduction particle, enhancing fibre
The dispersibility of dimension and other auxiliary agents is more preferable, and the combination property of composite is of a relatively high.
Being described in further detail the present invention below in conjunction with specific embodiment, these embodiments are it is not intended that limit this
Invent scope required for protection.
Embodiment 1
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 40 | Weight average molecular weight 4 × 105 |
| Carbon fiber length is fine | 5 | Fibre length 1mm, thermal conductivity is 90w/ (mk) |
| The short fibre of carbon fiber | 3 | Fibre length 0.15mm, thermal conductivity is 90w/ (mk) |
| Expanded graphite | 30 | Initial expansion temperature 260 DEG C；Particle diameter 200 mesh |
| Crystalline flake graphite | 3 | Particle diameter 2000 mesh |
| Glass fibre | 5 | Fibre length 50mm |
| Toughener (ethylene propylene diene rubber) | 10 | -- |
| Deca-BDE | 2.5 | -- |
| Antimony oxide | 0.5 | -- |
| Silane coupler (KH560) | 1 | -- |
Preparation technology:
Polyethylene and toughener granule are carried out in flour mill low temperature pulverizing (pulverizing temperature is-60 DEG C), to particle
Footpath is 100～150 μm, and pulverizing is the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at glass
In fiber, the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at scale
On graphite, and in mixer, mix 5min, the most standby.
Polyethylene, toughener, glass fibre and crystalline flake graphite after above-mentioned process is added in mixer, simultaneously by other
Raw material adds in mixer in the lump, mixes 5min, obtain mixture under the power of 3KW；
Carry out said mixture extruding, drawing and pelletize at 250 DEG C, prepare heat conduction composite polyethylene material.
Embodiment 2
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 30 | Weight average molecular weight 8 × 105 |
| Carbon fiber length is fine | 8 | Fibre length 3mm, thermal conductivity is 90w/ (mk) |
| The short fibre of carbon fiber | 5 | Fibre length 0.2mm, thermal conductivity is 90w/ (mk) |
| Expanded graphite | 35 | Initial expansion temperature 260. DEG C；Particle diameter 100. mesh |
| Crystalline flake graphite | 6 | Particle diameter 2000 mesh |
| Glass fibre | 5 | Fibre length 50mm |
| Toughener (ethylene-octene copolymer) | 7 | -- |
| Deca-BDE | 2.5 | -- |
| Antimony oxide | 0.5 | -- |
| Silane coupler (KH560) | 1 | -- |
Preparation technology:
Polyethylene and toughener granule are carried out in flour mill low temperature pulverizing (pulverizing temperature is-20 DEG C), to particle
Footpath is 100～150 μm, and pulverizing is the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at glass
In fiber, the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at scale
On graphite, and in mixer, mix 5min, the most standby.
Polyethylene, toughener, glass fibre and crystalline flake graphite after above-mentioned process is added in mixer, simultaneously by other
Raw material adds in mixer in the lump, mixes 5min, obtain mixture under the power of 3KW；
Carry out said mixture extruding, drawing and pelletize at 270 DEG C, prepare heat conduction composite polyethylene material.
Embodiment 3
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 25 | Weight average molecular weight 6 × 105 |
| Carbon fiber length is fine | 15 | Fibre length 5mm, thermal conductivity is 90w/ (mk) |
| The short fibre of carbon fiber | 5 | Fibre length 0.3mm, thermal conductivity is 90w/ (mk) |
| Expanded graphite | 35 | Initial expansion temperature 250 DEG C；Particle diameter 300 mesh |
| Crystalline flake graphite | 6 | Particle diameter 2000 mesh |
| Glass fibre | 5 | Fibre length 50mm |
| Toughener (ethylene-octene copolymer) | 5 | -- |
| Deca-BDE | 2.5 | -- |
| Antimony oxide | 0.5 | -- |
| Silane coupler (KH560) | 1 | -- |
Preparation technology:
Polyethylene and toughener granule are carried out in flour mill low temperature pulverizing (pulverizing temperature is-30 DEG C), to particle
Footpath is 100～150 μm, and pulverizing is the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at glass
In fiber, the most standby.
The silane coupler of 0.5 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at scale
On graphite, and in mixer, mix 5min, the most standby.
Polyethylene, toughener, glass fibre and crystalline flake graphite after above-mentioned process is added in mixer, simultaneously by other
Raw material adds in mixer in the lump, mixes 5min, obtain mixture under the power of 3KW；
Carry out said mixture extruding, drawing and pelletize at 200 DEG C, prepare heat conduction composite polyethylene material.
Embodiment 4
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 55 | Weight average molecular weight 4 × 105 |
| Carbon fiber length is fine | 23 | Fibre length 5mm, thermal conductivity is 80w/ (mk) |
| The short fibre of carbon fiber | 18 | Fibre length 0.2mm, thermal conductivity is 80w/ (mk) |
| Expanded graphite | 15 | Initial expansion temperature 260 DEG C；Particle diameter 100 mesh |
| Crystalline flake graphite | 35 | Particle diameter 2000 mesh |
| Glass fibre | 0 | -- |
| Toughener | 0 | -- |
| Deca-BDE | 0 | -- |
| Antimony oxide | 0 | -- |
| Silane coupler | 0 | -- |
Preparation technology:
Polyethylene is carried out in flour mill low temperature pulverizing (pulverizing temperature is-60 DEG C), is 100～150 μ to grain diameter
M, pulverizing is the most standby.
Polyethylene after above-mentioned process is added in mixer, other raw materials is added in mixer in the lump, at 3KW simultaneously
Power under mix 5min, obtain mixture；
Carry out said mixture extruding, drawing and pelletize at 280 DEG C, prepare heat conduction composite polyethylene material.
Embodiment 5
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 50 | Weight average molecular weight 4 × 105 |
| Carbon fiber length is fine | 20 | Fibre length 9mm, thermal conductivity is 90w/ (mk) |
| The short fibre of carbon fiber | 15 | Fibre length 0.15mm, thermal conductivity is 90w/ (mk) |
| Expanded graphite | 50 | Initial expansion temperature 250 DEG C；Particle diameter 300 mesh |
| Crystalline flake graphite | 3 | Particle diameter 5000 mesh |
| Glass fibre | 15 | Fibre length 50mm |
| Toughener (ethylene-octene copolymer) | 15 | -- |
| Tetrabromobisphenol A | 20 | -- |
| Sodium antimonate | 6 | -- |
| Silane coupler (KH560) | 3 | -- |
Preparation technology:
Polyethylene and toughener granule are carried out in flour mill low temperature pulverizing (pulverizing temperature is-60 DEG C), to particle
Footpath is 100～150 μm, and pulverizing is the most standby.
The silane couplers of 2 parts are diluted in ethanol the solution that concentration is 3wt%, by this spray solution in glass fibers
In dimension, the most standby.
The silane coupler of 1 part is diluted in ethanol the solution that concentration is 2wt%, by this spray solution at scale stone
Mo Shang, and in mixer, mix 5min, the most standby.
Polyethylene, toughener, glass fibre and crystalline flake graphite after above-mentioned process is added in mixer, simultaneously by other
Raw material adds in mixer in the lump, mixes 5min and obtain mixture under the power of 3KW；
Carry out said mixture extruding, drawing and pelletize at 270 DEG C, prepare heat conduction composite polyethylene material.
Embodiment 6
The present embodiment is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
Preparation technology:
Polyethylene and toughener granule are carried out in flour mill low temperature pulverizing (pulverizing temperature is-60 DEG C), to particle
Footpath is 100～150 μm, and pulverizing is the most standby.
The silane coupler of 0.3 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at glass
In fiber, the most standby.
The silane coupler of 0.2 part is diluted in ethanol the solution that concentration is 1wt%, by this spray solution at scale
On graphite, and in mixer, mix 5min, the most standby.
Polyethylene, toughener, glass fibre and crystalline flake graphite after above-mentioned process is added in mixer, simultaneously by other
Raw material adds in mixer in the lump, mixes 5min, obtain mixture under the power of 3KW；
Carry out said mixture extruding, drawing and pelletize at 240 DEG C, prepare heat conduction composite polyethylene material.
Comparative example 1
This comparative example is prepared for a kind of heat conduction composite polyethylene material.
Prepare raw material:
| Raw material | Consumption (g) | Parameter |
| Polyethylene | 25 | Weight average molecular weight 3 × 105 |
| Carbon fiber length is fine | 23 | Fibre length 0.6mm, thermal conductivity is 80w/ (mk) |
| The short fibre of carbon fiber | 18 | Fibre length 0.1mm, thermal conductivity is 80w/ (mk) |
| Expanded graphite | 0 | -- |
| Crystalline flake graphite | 0 | -- |
| Glass fibre | 0 | -- |
| Toughener (ethylene propylene diene rubber) | 0 | -- |
| Deca-BDE | 0 | -- |
| Antimony oxide | 0 | -- |
| Silane coupler (KH560) | 0 | -- |
Preparation technology:
Polyethylene is carried out in flour mill low temperature pulverizing (pulverizing temperature is-20 DEG C), is 100～150 μ to grain diameter
M, pulverizing is the most standby.
Polyethylene after above-mentioned process is added in mixer, simultaneously by carbon fiber length is fine and the short fibre of carbon fiber adds in the lump
In mixer, under the power of 3KW, mix 5min, obtain mixture；
Carry out said mixture extruding, drawing and pelletize at 280 DEG C, prepare heat conduction composite polyethylene material.
Heat conduction composite polyethylene material prepared in above-described embodiment 1 to 6 and comparative example 1 is carried out performance characterization.
Performance test, the impact property test of sample is measured according to GBT1043.1-2008, and is expressed as kJ/m2；
Sample Determination of conductive coefficients is carried out according to GB-T10297-1998, and is expressed as w/mk；Combustibility is tested according to UL94 standard
Test.Test result is as shown in table 1:
Table 1
From above data and description, it can be seen that add heat conducting fiber and heat conduction in base polyethylene simultaneously
Grain, it is possible to make composite have higher heat conductivility.Especially, after adding other auxiliary agents further, it is possible to carry further
The combination property of high composite so that it is have higher heat conductivility, shock resistance and fire resistance concurrently.Disclosure satisfy that high collection
Raw-material use requirement in one-tenth degree electronic device.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (18)
1. a heat conduction composite polyethylene material, it is characterised in that by weight, including the polyethylene of 15～50 parts, 4～35
The heat conducting fiber of part and the heat conduction particle of 23～80 parts；Wherein,
By weight, described heat conducting fiber includes the long fibre of 2～20 parts and the chopped fiber of 2～15 parts；Described long stapled
A length of 0.7～9mm, a length of the 0.15 of described chopped fiber～0.4mm；
By weight, described heat conduction particle includes the expanded graphite of 20～50 parts and the crystalline flake graphite of 3～30 parts；Described expansion
The initial expansion temperature of graphite is 250～280 DEG C；
The particle diameter of described expanded graphite is 100～300 mesh, and the particle diameter of described crystalline flake graphite is 1200～5000 mesh.
Composite the most according to claim 1, it is characterised in that the thermal conductivity of described heat conducting fiber > 80W/ (m K),
The hot strength of described heat conducting fiber > 700MPa.
Composite the most according to claim 1 and 2, it is characterised in that described heat conducting fiber is carbon fiber or metal fibre
Dimension.
Composite the most according to claim 3, it is characterised in that described heat conducting fiber is carbon fiber.
Composite the most according to claim 3, it is characterised in that by weight, also includes that the enhancing of 1～15 part is fine
Dimension.
Composite the most according to claim 5, it is characterised in that described reinforcing fiber is glass fibre.
Composite the most according to claim 5, it is characterised in that by weight, described heat conduction polyethylene composite wood
Material also includes: the fire retardant of 1～20 part, the fire retarding synergist of 0.5～6 part, the toughener of optional 3～15 parts and optional
The coupling agent of 0.5～3 part.
Composite the most according to claim 7, it is characterised in that described fire retardant is deca-BDE, decabrominated dipheny
One or more in ethane or tetrabromobisphenol A.
Composite the most according to claim 7, it is characterised in that described fire retarding synergist is antimony oxide, metaantimmonic acid
One or more in sodium or Firebrake ZB.
Composite the most according to claim 7, it is characterised in that described toughener is ethene-vinyl acetate copolymerization
One or more in thing, ethylene propylene diene rubber, ethylene-octene copolymer, SB.
11. composites according to claim 7, it is characterised in that described coupling agent is silane coupler.
The preparation method of the heat conduction composite polyethylene material described in 12. 1 kinds of claim 1, it is characterised in that include following step
Rapid:
S1, by weight, by the polyethylene of 15～50 parts, the heat conducting fiber of 4～35 parts, and the heat conduction particle of 23～80 parts
Mixer mixes, obtains mixture；
S2, carry out described mixture extruding, drawing and pelletize, obtain described heat conduction composite polyethylene material.
13. preparation methoies according to claim 12, it is characterised in that in described step S1, also include by weight
The reinforcing fiber of 1～15 part of meter adds in described mixer, with described polyethylene, described heat conducting fiber and described heat conduction particle
Jointly carry out the step mixed.
14. according to the preparation method described in claim 12 or 13, it is characterised in that in described step S1, also includes by weight
Amount part is counted the fire retarding synergist of the fire retardant of 1～20 part and 0.5～6 part and is added in described mixer, with described polyethylene, described
Heat conducting fiber, described heat conduction particle and optional described reinforcing fiber carry out the step mixed jointly.
15. preparation methoies according to claim 14, it is characterised in that in described step S1, are adding described polyethylene
Before entering in described mixer, by the toughener mixing of described polyethylene and 3～15 parts, and by mixture-60～-20 DEG C of temperature
Degree descends pulverizing to particle diameter below 150 μm.
16. preparation methoies according to claim 13, it is characterised in that in described step S1, by described crystalline flake graphite
Before adding in described mixer, also include the step that described crystalline flake graphite is carried out pretreatment；Described crystalline flake graphite is carried out
The step of pretreatment includes:
By weight, the coupling agent of 0.3～2 part is dissolved in ethanol, is configured to the first mixing that concentration is 1～3wt% molten
Liquid, sprays described first mixed solution to described crystalline flake graphite, and mixes in mixer, takes out and forms pre-place after drying
The described crystalline flake graphite of reason.
17. preparation methoies according to claim 14, it is characterised in that in described step S1, by described reinforcing fiber
Before adding in described mixer, also include the step that described reinforcing fiber is carried out pretreatment；Described reinforcing fiber is carried out
The step of pretreatment includes:
By weight, the coupling agent of 0.2～1 part is dissolved in ethanol, is configured to the second mixing that concentration is 1～3wt% molten
Liquid, sprays described second mixed solution to described reinforcing fiber, after drying, forms the described reinforcing fiber of pretreatment.
18. preparation methoies according to claim 12, it is characterised in that in described step S2, are carried out described mixture
During extrusion, extrusion temperature is 200～270 DEG C.
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| CN104356490B (en) * | 2014-12-06 | 2017-06-13 | 哈尔滨理工大学 | Heat conductive insulating composite polyolefine material and preparation method thereof |
| CN104893120A (en) * | 2015-06-09 | 2015-09-09 | 苏州圣谱拉新材料科技有限公司 | High-strength high-heat-conductivity composite material |
| CN105504547B (en) * | 2016-01-12 | 2018-08-17 | 赵继洁 | Graphite-based composite high-molecular thermo electric material, preparation method and its usage |
| CN108735346B (en) * | 2018-06-21 | 2020-05-26 | 珠海安润普科技有限公司 | Fatigue-resistant conductive composite material and preparation method thereof |
| WO2020158913A1 (en) * | 2019-01-31 | 2020-08-06 | 積水テクノ成型株式会社 | Resin molded body |
| CN115216076B (en) * | 2022-08-29 | 2023-12-19 | 中国科学院长春应用化学研究所 | Heat-conducting polyethylene pipe and preparation method thereof |
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Effective date of registration: 20170914 Address after: 100084, building 9, building 1, Zhongguancun East Road, Beijing, Haidian District, 04-09A Co-patentee after: Tianjin Huachuang Ruifeng air conditioning equipment Co. Patentee after: Beijing SinoRefine Air Conditioning Technology Co., Ltd. Address before: 100084, building 9, building 1, Zhongguancun East Road, Beijing, Haidian District, 04-09A Patentee before: Beijing SinoRefine Air Conditioning Technology Co., Ltd. |