CN107915974A - Heat-conductive resin composition and preparation method thereof - Google Patents
Heat-conductive resin composition and preparation method thereof Download PDFInfo
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- CN107915974A CN107915974A CN201610878251.9A CN201610878251A CN107915974A CN 107915974 A CN107915974 A CN 107915974A CN 201610878251 A CN201610878251 A CN 201610878251A CN 107915974 A CN107915974 A CN 107915974A
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Abstract
The present invention relates to heat-conductive resin composition and preparation method thereof, mainly solves the problems, such as that high heat conduction amount of filler existing in the prior art causes the comprehensive mechanical property of material to be deteriorated.The present invention is by using heat-conductive resin composition, including following components in terms of parts by weight：A) 40~80 parts of thermoplastic resin；B) 10~45 parts of heat conduction filler composition；C) 0.01~1 part of interface modifier；D) 0.1~10 part other fillers；Wherein, the heat conduction filler composition is the technical solution of at least one of the heat filling with length/diameter ratio >=1 or the heat filling with length/thickness than >=1, preferably solves the problems, such as this, available for industrialized production.
Description
Technical field
The invention belongs to polymer composite, is related to a kind of heat-conductive resin composition and preparation method thereof.The heat conduction
Resin combination is suitable for electric, electronics and thermal component.
Background technology
Heat Conduction Material such as is commonly applied to exchange heat, radiates, is electric the industry.In recent years, electronic and electrical equipment lightweight, small
Type and high performance trend are obvious, and the caloric value of its heat generating components also has increase tendency.Excessive heat reduces the property of product
Can, heat conduction is distributed in time most important.Improve the heat dissipation performance of heating device, issued high thermal conductivity and there is cost
The Heat Conduction Material of advantage is particularly urgent.
Compared with the materials such as traditional metal, ceramics, heat-conducting plastic has lot of advantages：Heat dissipation uniformly, low thermal resistance, it is low into
This, the selection of convenient, a variety of matrix resin of machine-shaping, design freedom is high, 3 D complex degree is high, light, thermal coefficient of expansion
It is low, molding shrinkage is low, operating temperature is low, increase convective surface, file is integrated etc., heat-conducting plastic has become domestic and international at present
The research and development focus of heat sink material.Since the heat conductivility of high molecular material is very poor, only about 0.2Wm-1·K-1, so people carry
Go out using high molecular material as matrix to prepare conductive plastic material.Preparing heat-conducting plastic mainly has two methods：One kind is with change
Learn synthetic method, i.e. Intrinsical, high molecular material of the synthesis with high conjugation degree, high-crystallinity or high-orientation, as polyacetylene,
Polyphenylene sulfide, polythiophene etc..But its preparation process is cumbersome, difficulty is big, of high cost, it is difficult to realizes industrialized production.Two
It is the inorganic filler of filling Heat Conduction Material, such as metal, high heat conduction in polymer (such as polyolefin, polyester, nylon).The latter
Method is simple, efficient, and the work to filling-modified research is more both at home and abroad, such as RTP, DSM, Mitsubishi, SABIC, precious profit
The auspiciousness science and technology of agate, silver, fly the company such as illustrious and influential.
The external multinomial patented invention on heat-conducting plastic exploitation, such as US 20120217434, US 20150069290, JP
2014231538th, WO 2009043850 etc., is mainly produced, there is provided the series of excellent high thermal conductivity is led using completion method
Thermoplastic materials product, but the ratio of used heat filling and auxiliary agent is higher, causes manufacturing cost height.Sumitomo Chemical strain formula
Commercial firm patent CN 101041719A disclose by the filler such as thermoplastic resin and granulated alumina fibre be pre-mixed after, through squeeze
Go out the granulation of machine melt kneading, then product is obtained through injection moulding, the component as electronic unit, particularly requires thermal conductivity
Component.Heat-conducting plastic prepared by the patent has 2.7~5.0Wm-1·K-1Parallel thermal conductivity, 0.6~2.9Wm-1·K-1Vertical thermal conductivity.Ti Kena house journals of U.S. CN 102482449A, which are disclosed, fills out liquid crystal polymer and heat conduction
Material, glass fibre etc. mix, and 0.6~1.5Wm of thermal conductivity is obtained after Screw Extrusion-1·K-1Heat conductive resin composition,
For requiring the Electrical and Electronic shell of high heat conductor.Shanghai Jie Shijie new materials house journal CN 103965616A are reported
Heat is made by the blending of Screw Extrusion melt kneading in thermoplastic resin, heat-conducting resin masterbatch, boron carbide particle, coupling agent etc.
2.1~4.2Wm of conductance-1·K-1Heat-conducting resin.Due to it with the addition of substantial amounts of inorganic filler in resin after, its melt-flow
Performance will become very poor, and the related data report of the material performance is showed no in above-mentioned patent.In addition, reported in the patent
Heat filling ratio is higher used by the heat-conducting resin in road causes mechanical properties decrease, causes production cost higher, certain journey
Its application is limited on degree.
The content of the invention
The first technical problem to be solved by the present invention is that high heat conduction amount of filler existing in the prior art causes material
Comprehensive mechanical property be deteriorated the problem of, there is provided a kind of heat-conductive resin composition.The heat-conductive resin composition comprehensive performance obtains
Significantly improve, also with excellent mechanical property with preferable fluidity of molten and while heat conductivility, suitable for electrically,
Electronics and thermal component.
The second technical problem to be solved by the present invention is to provide the heat-conducting resin adaptable with solving one of technical problem
The preparation method of composition.The technical solution technique is simple, easy to operate so that the comprehensive performance of heat-conductive resin composition obtains
Significantly improve, also with excellent mechanical property with preferable fluidity of molten and while heat conductivility, suitable for electrically,
Electronics and thermal component.
To solve one of above-mentioned technical problem, the technical solution adopted by the present invention is as follows：A kind of heat-conductive resin composition, with
Parts by weight meter includes following components：
(A) 40~80 parts of thermoplastic resin；
(B) 10~45 parts of heat conduction filler composition；
(C) 0.01~1 part of interface modifier；
(D) 0.1~10 part other fillers；
Wherein, the heat conduction filler composition be selected from heat filling with length/diameter ratio >=1 or with length/
At least one of heat filling of thickness ratio >=1.The heat filling with length/diameter ratio >=1 is selected from fiber powdery
At least one of heat filling, chopped strand shape heat filling and long fine shape heat filling.Described has length/thickness ratio
>=1 heat filling is selected from least one of sheet heat filling.
In above-mentioned technical proposal, the thermoplastic resin be selected from polypropylene, polyester, nylon, polystyrene, styrene/
Acrylonitrile copolymer, phenylethylene/maleic anhydride copolymer, ABS, makrolon, polyphenylene oxide, polyphenylene sulfide, polyether-ether-ketone, liquid crystal
At least one of polymer.
In above-mentioned technical proposal, length/diameter ratio >=1, wherein, length be selected from >=20 μm, diameter be selected from 0.1~
20μm。
In above-mentioned technical proposal, the fiber powdery heat filling be selected from glass fiber powder, graphite powder, carbon nanotubes and
At least one of carbon fiber powder；The chopped strand shape heat filling is in short glass fiber and chopped carbon fiber
It is at least one；The long fine shape heat filling is selected from least one of glass fibre and carbon fiber.
In above-mentioned technical proposal, length/thickness ratio >=1, wherein, length is selected from 0.2~800 μm, and thickness is selected from
10~200nm.
In above-mentioned technical proposal, the sheet heat filling is selected from least one of graphite and graphene.
In above-mentioned technical proposal, it is described with certain length/diameter than heat filling or with certain length/thickness
The heat filling of ratio, can also carry out compounding use with other kinds of heat filling.With certain length/diameter than heat conduction
The mass ratio of filler or heat filling and other kinds of heat filling with certain length/thickness ratio is 99:1~1:99.
Wherein, other described fillers are selected from spherical aluminium oxide, magnesia, zinc oxide, silica, aluminium nitride, silicon nitride, carbonization
At least one of silicon；The particle diameter of the spherical heat filling is 20~2000 mesh.
In above-mentioned technical proposal, the interface modifier is selected from silanes modifying agent, polyesters modifying agent, titanate ester
At least one of modifying agent, more preferably from silanes modifying agent, such as aminopropyl triethoxysilane, γ-glycidyl ether oxygen
At least one of propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane.
In above-mentioned technical proposal, the heat-conductive resin composition can also include processing aid, processing aid choosing
From antioxidant and plasticiser；The antioxidant is selected from polyphenol kind antioxidant, such as four [β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) propionic acid] pentaerythritol ester, at least one of β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid；Institute
The plasticiser stated is selected from least one of white oil, paraffin wax.
To solve the two of above-mentioned technical problem, the technical solution adopted by the present invention is as follows：A kind of heat-conductive resin composition
Preparation method, comprises the following steps：
(1) the desired amount of heat filling is subjected to surface modification treatment with the desired amount of interface modifier, obtained described
Heat conduction filler composition；
(2) the desired amount of heat conduction filler composition is mixed with thermoplastic resin, the processing aid of drying process in one
Mixed in device such as high-speed mixer, import in screw extruder and melted, mediate, extrude, being granulated, thermoplasticity heat conduction is made
Resin combination.Preferable screw extruder is double screw extruder.
To solve the two of above-mentioned technical problem, the technical solution adopted by the present invention is as follows：A kind of heat-conductive resin composition
Preparation method, it is further comprising the steps of：
(1) the desired amount of heat filling is subjected to surface modification treatment with the desired amount of interface modifier, obtained described
Heat conduction filler composition；
(2) it is the desired amount of heat conduction filler composition and the thermoplastic resin of drying process, processing aid is mixed without high speed
Mixed in conjunction machine, directly metering, which is imported in a screw extruder, is melted, mediates, extrude, being granulated, and thermoplasticity heat conduction is made
Resin combination.Preferable screw extruder is double screw extruder.
Invention method is accompanied by boundary modification by selecting the heat conduction filler composition of special size and shape
Agent, is entered in base resin material by melt blending, obtains also having while having higher thermal conductivity and melt flowability
There is the heat-conductive resin composition of excellent mechanical mass performance, and reduce production cost, beneficial to realizing industrialized production.The present invention
The key of method is collocation, ratio, feed way, the selection of thermoplastification processing conditions of the heat filling raw material of different structure
Deng.
Using the heat filling component of the heat-conductive resin composition prepared by the present invention at 30 parts, parallel thermal conductivity exists
3.0W·m-1·K-1Above, vertical thermal conductivity is in 0.9Wm-1·K-1More than, at the same material had melt flowability,
High modulus and toughness, excellent combination property, achieves preferable technique effect.
The performance of the present invention is determined by the following procedure：
Density measurement：Sample is placed in ALFA MIRAGE SD-200L electronic densitometers, measures the density of Heat Conduction Material.
Melt index (MFR) measures：By ASTM D1238 standards, measured using LLOYD DAVENPORT fusion index instruments.
Heat resistance is tested：Dimension card is measured using Italy's CEAST companies Wei Ka thermal deformation analyzers by 306 standards of ISO
Softening point；Heat distortion temperature is measured using Italy's CEAST companies Wei Ka thermal deformation analyzers by ISO 75-2 standards.
Bending property is tested：By 178 standards of ISO using Instron Company Materials of U.S. testing machine measure.
Notched impact properties is tested：By 179 standards of ISO using CEAST companies of Italy Apparatus for Impacting at low-temp measure.
Heat conductivility is tested：Surveyed by ASTM E1461 standards using NETZSCH companies of Germany laser thermal conductivity coefficient measurement instrument
It is fixed.
Below by specific embodiment, the present invention will be further elaborated.
Embodiment
【Embodiment 1】
Heat filling is surface-treated：Weigh 20 parts of chopped carbon fiber (10 μm of length 5mm, diameter) and 10 parts of silane coupling agents
The ethanol solution of concentration 2.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry,
Obtain heat conduction filler composition A1.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 80 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A1, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters
1010 0.8 parts, 0.8 part of white oil, are placed in homogenizer and are sufficiently mixed 2 minutes.Mixed material is imported into double screw extruder
Middle melting extrusion, granulation obtain heat-conductive resin composition B1.The temperature of 1~9 section of double screw extruder and die orifice is followed successively by 220
DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 270 DEG C, 150 revs/min of screw speed, melt
Temperature is 278 DEG C, and melt pressure is 20~32bar, 25~38Hz of moment of torsion.
Injection molded test：Dried B1 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B1.
【Embodiment 2】
Heat filling is surface-treated：Weigh 40 parts of chopped carbon fiber (10 μm of length 5mm, diameter) and 10 parts of silane coupling agents
The ethanol solution of concentration 4.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry,
Obtain heat conduction filler composition A2.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 60 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A2,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B2.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 281 DEG C, melt pressure is 27~41bar, 30~33Hz of moment of torsion.
Injection molded test：Dried B2 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B2.
【Embodiment 3】
Heat filling is surface-treated：Weigh 30 parts of chopped carbon fiber (10 μm of length 5mm, diameter), flake graphite alkene YH5
(particle diameter D50：150 μm, thickness 80nm) ethanol solutions of 5 parts and 10 parts of silane coupled agent concentrations 3.5% fills in stainless steel ware
Divide and be stirred, when drying 4 is small at 100 DEG C after naturally dry, obtain heat conduction filler composition A3.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 65 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A3,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B3.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 283 DEG C, melt pressure is 28~42bar, 31~39Hz of moment of torsion.
Injection molded test：Dried B3 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B3.
【Embodiment 4】
Heat filling is surface-treated：Weigh 25 parts of chopped carbon fiber (10 μm of length 5mm, diameter), flake graphite alkene YH5
(particle diameter D50：150 μm, thickness 80nm) ethanol solutions of 5 parts and 10 parts of silane coupled agent concentrations 3.0% fills in stainless steel ware
Divide and be stirred, when drying 4 is small at 100 DEG C after naturally dry, obtain heat conduction filler composition A4.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A4,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B4.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 280 DEG C, melt pressure is 22~33bar, 22~35Hz of moment of torsion.
Injection molded test：Dried B4 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B4.
【Embodiment 5】
Heat filling is surface-treated：Weigh 30 parts of chopped carbon fiber (10 μm of length 5mm, diameter) and 10 parts of silane coupling agents
The ethanol solution of concentration 3.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry,
Obtain heat conduction filler composition A5.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 59.5 parts, styrene/
10.5 parts of copolymer-maleic anhydride M14 under vacuum condition, when drying process 6 is small at 105 DEG C, 60 DEG C after, with A5,
1010 0.8 parts, 0.8 part of white oil, are placed in homogenizer and are sufficiently mixed 2 minutes.Mixed material is imported into double screw extruder
Middle melting extrusion, granulation obtain heat-conductive resin composition B5.The temperature of 1~9 section of double screw extruder and die orifice is followed successively by 220
DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 270 DEG C, 150 revs/min of screw speed, melt
Temperature is 275 DEG C, and melt pressure is 16~27bar, 17~27Hz of moment of torsion.
Injection molded test：Dried B5 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B5.
【Embodiment 6】
Heat filling is surface-treated：It is dense with 10 parts of silane coupling agents to weigh 30 parts of graphite powder I (10 μm of length, 5 μm of thickness)
The ethanol solution of degree 3.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry, is obtained
To heat conduction filler composition A6.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A6,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B6.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 279 DEG C, melt pressure is 22~36bar, 21~33Hz of moment of torsion.
Injection molded test：Dried B6 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B6.
【Embodiment 7】
Heat filling is surface-treated：It is dense with 10 parts of silane coupling agents to weigh 30 parts of graphite powder II (30 μm of length, 8 μm of thickness)
The ethanol solution of degree 3.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry, is obtained
To heat conduction filler composition A7.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A7,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B7.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 279 DEG C, melt pressure is 22~36bar, 21~33Hz of moment of torsion.
Injection molded test：Dried B7 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B7.
【Embodiment 8】
Heat filling is surface-treated：Weigh 15 parts of graphite powder I (10 μm of length, 5 μm of thickness), graphite powder II (30 μm of length,
8 μm of thickness) ethanol solutions of 15 parts and 10 parts of silane coupled agent concentrations 3.0% is thoroughly mixed in stainless steel ware, from
When drying 4 is small at 100 DEG C after so drying, heat conduction filler composition A8 is obtained.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A8,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B8.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 287 DEG C, melt pressure is 28~39bar, 30~37Hz of moment of torsion.
Injection molded test：Dried B8 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B8.
【Embodiment 9】
Heat filling is surface-treated：Weigh 30 parts of fiber graphite powder CF-200 (80 μm of length, 5 μm of diameter) and 10 parts of silicon
The ethanol solution of alkane coupling agent concentrations 3.0% is thoroughly mixed in stainless steel ware, is done after naturally dry at 100 DEG C
It is dry 4 it is small when, obtain heat conduction filler composition A9.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A9,1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition B9.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 287 DEG C, melt pressure is 28~39bar, 30~37Hz of moment of torsion.
Injection molded test：Dried B9 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B9.
【Embodiment 10】
Heat filling is surface-treated：It is dense with 10 parts of silane coupling agents to weigh 30 parts of fiber graphite powder CF-200 (200 mesh)
The ethanol solution of degree 3.0% is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry, is obtained
To heat conduction filler composition A9.
The preparation of thermoplasticity heat-conductive resin composition：By polycarbonate pellet (melt index 12.3g10min-1) 70 parts
When drying process 6 is small under 105 DEG C, vacuum condition, twin-screw is imported by loss-in-weight feeder respectively with A9,1,010 0.8 parts and is squeezed
Go out in machine, 0.8 part of white oil is imported in double screw extruder by HLB-1008 piston pump with constant flow, through melting, mediating, extruding, making
Grain obtains thermoplasticity heat-conductive resin composition B10.The temperature of 1~9 section of double screw extruder and die orifice be followed successively by 220 DEG C, 240
DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature
For 285 DEG C, melt pressure is 24~35bar, 28~33Hz of moment of torsion.
Injection molded test：Dried B10 is molded into by standard batten, injection molding machine 1~3 using German BOY M55 injection molding machines
Section and film mouth temperature are respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C, and 60 DEG C of mold temperature, is placed in Bluepard BPS-
When placement 24 is small in 100CB climatic chambers (23 DEG C of temperature, relative humidity 50%).
The all-round property testing of thermoplasticity heat-conductive resin composition B10 the results are shown in Table 1.
【Embodiment 11】
Heat filling is surface-treated：Weigh flake graphite alkene YH5 (particle diameter D50：150 μm, thickness 80nm) 5 parts, flake graphite
Alkene YH1 (particle diameter D50：20 μm, thickness 80nm) 2.5 parts, 22.5 parts of fiber graphite powder CF-200 (80 μm of length, 5 μm of diameter) with
The ethanol solution of 10 parts of silane coupled agent concentrations 3.0% is thoroughly mixed in stainless steel ware, then at 100 after naturally dry
When drying 4 is small at DEG C, heat conduction filler composition A10 is obtained.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with A10,1,010 1.6 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2
Minute.Said mixture material is imported into melting extrusion in extruder, granulation obtains heat-conductive resin composition B10.Twin-screw extrusion
The temperature of 1~9 section of machine and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 288 DEG C, melt pressure is 27~42bar, 26~42Hz of moment of torsion.
Injection molded test：Dried B10 is molded into by standard batten, injection molding machine 1~3 using German BOY M55 injection molding machines
Section and film mouth temperature are respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C, and 60 DEG C of mold temperature, is placed in Bluepard BPS-
When placement 24 is small in 100CB climatic chambers (23 DEG C of temperature, relative humidity 50%).
1 the results are shown in Table to the all-round property testing of heat-conductive resin composition B10.
【Comparative example 1】
Injection molded test：By polycarbonate pellet C1 (melting means 12.3g10min-1) it is dry under 105 DEG C, vacuum condition at
Manage 6 it is small when after, standard batten is molded into using German BOY M55 injection molding machines, 1~3 section of injection molding machine and film mouth temperature are distinguished
For 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB climatic chamber (temperature
23 DEG C, relative humidity 50%) in place 24 it is small when.
2 the results are shown in Table to the all-round property testing of C1.
【Comparative example 2】
Heat filling is surface-treated：Weigh 5 parts of graphite powder I (10 μm of length, 5 μm of thickness), graphite powder II (30 μm of length,
8 μm of thickness) ethanol solutions of 5 parts and 10 parts of silane coupled agent concentrations 1.0% is thoroughly mixed in stainless steel ware, and it is natural
When drying 4 is small at 100 DEG C after drying, heat conduction filler composition D is obtained.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 90 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with D, 1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition C2.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 278 DEG C, melt pressure is 23~32bar, 26~30Hz of moment of torsion.
Injection molded test：Dried C2 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
2 the results are shown in Table to the all-round property testing of heat-conductive resin composition C2.
【Comparative example 3】
Heat filling is surface-treated：Weigh 10 parts of ball-aluminium oxide (150 mesh) and 10 parts of silane coupled agent concentrations 1.0%
Ethanol solution is thoroughly mixed in stainless steel ware, when drying 4 is small at 100 DEG C after naturally dry, is obtained heat conduction and is filled out
Feed composition E.
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 90 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with E, 1,010 0.8 parts, 0.8 part of white oil, it is placed in homogenizer and is sufficiently mixed 2 points
Clock.Mixed material is imported into melting extrusion in double screw extruder, granulation obtains heat-conductive resin composition C3.Double screw extruder
The temperature of 1~9 section and die orifice be followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280
DEG C, 270 DEG C, 150 revs/min of screw speed, melt temperature be 288 DEG C, melt pressure is 35~55bar, 32~40Hz of moment of torsion.
Injection molded test：Dried C3 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
2 the results are shown in Table to the all-round property testing of heat-conductive resin composition C3.
【Comparative example 4】
The preparation of heat-conductive resin composition：By polycarbonate pellet (melting means 12.3g10min-1) 70 parts in 105 DEG C, it is true
After when drying process 6 is small under empty condition, with flake graphite alkene YH5 (particle diameter D50：150 μm, thickness 80nm) 5 parts, flake graphite alkene
YH1 (particle diameter D50：20 μm, thickness 80nm) 2.5 parts, 22.5 parts of fiber graphite powder CF-200 (80 μm of length, 5 μm of diameter) with
0.3 part of silane coupling agent, 1,010 1.6 parts, 0.8 part of white oil, are placed in homogenizer and are sufficiently mixed 2 minutes.By above-mentioned mixing
Material imports melting extrusion in extruder, and granulation obtains thermoplasticity heat-conductive resin composition C4.1~9 section of double screw extruder and
The temperature of die orifice is followed successively by 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 280 DEG C, 270 DEG C,
150 revs/min of screw speed, melt temperature are 288 DEG C, and melt pressure is 27~42bar, 26~42Hz of moment of torsion.
Injection molded test：Dried C4 is molded into by standard batten, 1~3 section of injection molding machine using German BOY M55 injection molding machines
It it is respectively 280 DEG C, 290 DEG C, 300 DEG C and 290 DEG C with film mouth temperature, 60 DEG C of mold temperature, is placed in Bluepard BPS-100CB
When placement 24 is small in climatic chamber (23 DEG C of temperature, relative humidity 50%).
2 the results are shown in Table to the all-round property testing of heat-conductive resin composition C4.
Contrasted from above-described embodiment and comparative example, the thermoplasticity heat-conductive resin composition prepared by the present invention is heat-resisting
Performance, mechanics, heat conductivility and melt flowability are preferable, especially select to obtain after two kinds of different heat fillings are composite modified
Heat-conductive resin composition comprehensive performance it is best, such as two kinds of flake graphite alkene, the compounding of fiber graphite powder.
Invention method is accompanied by modification and helps by selecting the conductive particle composition of special construction (size, shape)
Agent, is entered in base resin material by melt blending, obtains the thermoplastic with higher thermal conductivity, mechanics and melt flowability
Property heat-conductive resin composition, and reduce production cost, beneficial to realizing industrialized production.
The comprehensive performance of heat-conductive resin composition in 1 embodiment 1~11 of table
The comprehensive performance of heat-conductive resin composition in 2 comparative example 1~4 of table
Claims (9)
- A kind of 1. heat-conductive resin composition, including following components in terms of parts by weight：(A) 40~80 parts of thermoplastic resin；(B) 10~45 parts of heat conduction filler composition；(C) 0.01~1 part of interface modifier；(D) 0.1~10 part other fillers；Wherein, the heat conduction filler composition is for the heat filling with length/diameter ratio >=1 or with length/thickness ratio >=1 At least one of heat filling；The heat filling with length/diameter ratio >=1 be selected from fiber powdery heat filling, At least one of chopped strand shape heat filling and long fine shape heat filling.It is described that there is heat conduction of the length/thickness than >=1 to fill out Material is selected from least one of sheet heat filling.
- 2. heat-conductive resin composition according to claim 1, it is characterised in that the thermoplastic resin is selected from polypropylene, gathers Ester, nylon, polystyrene, styrene/acrylonitrile copolymer, phenylethylene/maleic anhydride copolymer, ABS, makrolon, polyphenyl At least one of ether, polyphenylene sulfide, polyether-ether-ketone, liquid crystal polymer.
- 3. heat-conductive resin composition according to claim 1, it is characterised in that the heat conduction with length/diameter ratio >=1 The length of filler is selected from >=20 μm, and diameter is selected from 0.1~20 μm.
- 4. according to the heat-conductive resin composition of claim 1 or 3, it is characterised in that the fiber powdery heat filling is selected from glass At least one of glass fiber powder, graphite powder, carbon nanotubes and carbon fiber powder；The chopped strand shape heat filling, which is selected from, to be chopped At least one of glass fibre and chopped carbon fiber；The long fine shape heat filling in glass fibre and carbon fiber extremely Few one kind.
- 5. heat-conductive resin composition according to claim 1, it is characterised in that described that there is heat conduction of the length/thickness than >=1 The length of filler is selected from 0.2~800 μm, and thickness is selected from 10~200nm.
- 6. according to the heat-conductive resin composition of claim 1 or 5, it is characterised in that the sheet heat filling be selected from graphite or At least one of graphene.
- 7. heat-conductive resin composition according to claim 1, it is characterised in that the interface modifier is modified selected from silanes At least one of agent, polyesters modifying agent, titanate ester modifying agent.
- 8. the preparation method of any heat-conductive resin composition of claim 1~7, comprises the following steps：(1) the desired amount of heat filling is subjected to surface modification treatment with the desired amount of interface modifier, obtains the heat conduction Fill composition；(2) by the desired amount of heat conduction filler composition and the thermoplastic resin of drying process, processing aid in high-speed mixer Mixing, imports in screw extruder and is melted, mediate, extrude, being granulated, and heat-conductive resin composition is made.
- 9. the preparation method of any thermoplasticity heat-conductive resin composition of claim 1~7, comprises the following steps：(1) the desired amount of heat filling is subjected to surface modification treatment with the desired amount of interface modifier, obtains the heat conduction Fill composition；(2) by the desired amount of heat conduction filler composition and the thermoplastic resin of drying process, processing aid without high-speed mixer Mixing, directly metering, which are imported in screw extruder, to be melted, mediates, extrudes, being granulated, and heat-conductive resin composition is made.
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| CN110564059A (en) * | 2019-09-19 | 2019-12-13 | 常州大学 | high-thermal-conductivity polypropylene composite material and preparation method thereof |
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Application publication date: 20180417 |