CN108285573A - A kind of high heat conductive insulating thermoplastic polymer and preparation method - Google Patents
A kind of high heat conductive insulating thermoplastic polymer and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of high heat conductive insulating thermoplastic polymer and preparation methods.The thermoplastic polymer is to be blended by the raw material including following components and obtained:100 parts by weight of thermoplastic resin;5~80 parts by weight of heat-conductive insulation filling;Heat-conductive insulation filling is heat conduction powder and its is surface coated with melanin structure thermally conductive insulating layer;Heat conduction powder is metal simple-substance or carbon-based powder;It is that metal heat-conducting powder is modified gained by least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance by surface with melanin structure thermally conductive insulating layer.Preparation method includes:The high heat conductive insulating thermoplastic polymer is made after pressing the dosage melt blending in the component.The composition of the present invention meets good heat conductivility and electrical insulation capability simultaneously, well solves thermal conductivity and insulation performance matching problem that high-power component work is encountered, can meet performance requirement of the current electronic product to heat conductive insulating high molecular material.
Description
Technical field
The present invention relates to thermoplastic resin technical fields, further say, are to be related to a kind of high heat conductive insulating thermoplastic poly
Close object and preparation method.
Background technology
Heat Conduction Material has in national defense industry and national economy every field to be widely applied very much.It is traditional to lead
Heat, conductive material refer to metal such as Au, Ag, Cu, Al, Mg etc., metal oxide such as A1 more2O3, MgO, BeO, NiO etc., nitride metal
Object such as AlN, Si3N4, BN etc. and other nonmetallic materials such as graphite and carbon black etc..With industrial production and science and technology it is fast
Speed development, people propose update, higher requirement to Heat Conduction Material, in addition to thermal conductivity, it is desirable to which material has excellent synthesis
Performance is for example light, easy technology, excellent in mechanical performance, resistant to chemical etching etc., and due to the fast development of modern information industry,
There is ultra-thin, light, digitlization, multifunction, networking direction to develop electronic equipment and expresses very high expectation.
High molecular material is since with the molding of light, resistant to chemical etching, easy processing, electrical insulation capability is excellent, mechanics and anti-
The excellent features such as fatigue behaviour is excellent start to permeate to these fields, and gradually play important role in this field.
However, since high molecular material is insulator, and thermal conductivity is extremely low, greatly limits its answering in these fields
With.Therefore, it develops with high thermal conductivity, and the high molecular material of excellent combination property is the heat studied in recent years
Point, and notable achievement is achieved, further widen application field of the high molecular material in terms of heat conduction.Especially in recent years, high
Development of information industry, such as widely used high heat dissipation interface material and encapsulating material, electromagnetism in electric appliance, field of microelectronics
The components such as shielding, the widely used power tube of electronic information field, integrated package, heat pipe, integrated circuit, copper-clad base plate, plastics
Application on these high-end information product accessories will be towards high power, densification, highly integrated, the directions such as rapid heat dissipation
Development, this development for high heat conduction high molecular material in new field provide the stage of bigger.
High molecular material thermal conductivity is poor, this is because it transmits the orderly crystal of required uniform compact without heat
Structure or charge carrier, to provide the propagation and diffusion of heat.Currently, there are mainly two types of ways for the thermal conductivity of raising high molecular material
Diameter:First, the structural type heat-conducting polymer material with thermal conductive resin is prepared, such as polyacetylene with a conjugated structure, polyphenyl
The materials such as amine, polypyrrole, or the crystallinity of polymer is improved, heat conduction purpose is realized by phonon thermal conduction mechanism.However, this
Requirement of the kind method to equipment, process conditions is all very high, it is more difficult to realize industrialized production.Second is that having by being added into matrix
The method of the filler of high-termal conductivity prepares filled-type polymer composite.This method and process is simple, for the former
It is more prone to control and realizes, cost is relatively low, is current raising high molecular material thermal conductivity so being adopted extensively by people
Main research means.
Invention content
To solve the problem in the prior art, the present invention provides a kind of high heat conductive insulating thermoplastic polymer and systems
Preparation Method.The composition meets good heat conductivility and electrical insulation capability simultaneously, and well solving high-power component work is
The thermal conductivity and insulation performance matching problem encountered, can meet performance of the current electronic product to heat conductive insulating high molecular material
It is required that.
An object of the present invention is to provide a kind of high heat conductive insulating thermoplastic polymer.
Raw material including following components is blended and obtains:
Each component is counted in parts by weight,
100 parts by weight of thermoplastic resin;
5~80 parts by weight of heat-conductive insulation filling;
The heat-conductive insulation filling is heat conduction powder and its is surface coated with melanin structure thermally conductive insulating layer;
The heat conduction powder is metal simple-substance or carbon-based powder;
It is described that have melanin structure thermally conductive insulating layer be heat conduction powder by DOPA, dopamine, Dopamine hydrochloride, tyrosine
At least one of substance by surface be modified gained.
It is preferred that:
The metal simple-substance is Au, Ag, Cu, Mg, Al, Fe, Ni, Be, Ca, Pt or Zn;The carbon-based powder is graphite, carbon
Fiber, carbon nanotube, fullerene, graphene or amorphous carbon;
The shape of the heat conduction powder includes granular, sheet, spherical shape or threadiness.Wherein linear heat conduction powder includes Cu nanometers
Line, Ag nano wires, carbon nanotube etc.;Sheet heat conduction powder includes Cu nanometer sheets, Ag nanometer sheets, Au nanometer sheets, graphene etc.;
A diameter of 20~500nm of linear heat conduction powder, length are 10~120 μm, and draw ratio is between 100~1000;
Spherical or granular heat conduction powder diameter is in 10nm~50 μm;
For sheet heat conduction powder length in 200nm~100 μm, thickness is nanoscale.
The heat-conductive insulation filling is prepared by method comprising the following steps:
A. heat conduction powder dispersion liquid is prepared;
B. at least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance are added to heat conduction powder dispersion liquid
In, it polymerize and the heat-conductive insulation filling is made.
Wherein, preferably:
In step a, deionized water and heat conduction powder amount ratio are 1 in heat conduction powder dispersion liquid:(0.001~0.05);
In step b, the dosage of at least one of heat conduction powder and DOPA, dopamine, Dopamine hydrochloride, tyrosine substance
Than being 1:(0.05~1).
The method for specifically including following steps is prepared:
Ultrasonic disperse is added in deionized water to uniformly obtaining heat conduction powder dispersion liquid in heat conduction powder by a;
At least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance is added in b in above-mentioned solution, with three (hydroxyls
Methyl) aminomethane (Tris) adjust solution ph be 8~10, at 45 DEG C~70 DEG C react 5~for 24 hours, pass through after reaction
Centrifugation, it is dry after washing, the heat-conductive insulation filling is made.
The thermoplastic resin is preferably polyethylene, high density polyethylene (HDPE), polypropylene, polystyrene, polyvinyl chloride, poly- carbon
Acid esters, nylon 6, nylon66 fiber, thermoplastic polyurethane, Acrylonitrile Butadiene-Styrene copolymer, polymethyl methacrylate, polyethylene terephthalate
At least one of ester, polybutylene terephthalate (PBT), thermoplastic polyimide.
Preferred amount ranges:
The thermoplastic resin is 100 parts by weight meters, and the graininess heat filling is 40~80 parts by weight, linear heat conduction
Filler is 5~30 parts by weight, and sheet heat filling is 5~30 parts by weight.
The second object of the present invention is to provide a kind of preparation method of high heat conductive insulating thermoplastic polymer.
Including:
The high heat conductive insulating thermoplastic polymer is made after pressing the dosage melt blending in the component.
Following technical scheme specifically can be used in the present invention:
A kind of high heat conductive insulating thermoplastic polymer, including the raw material of following components are blended and obtain:
Each component is counted in parts by weight,
100 parts by weight of thermoplastic resin;
5~80 parts by weight of heat-conductive insulation filling;
The thermoplastic polymer includes polyethylene (PE), high density polyethylene (HDPE) (HDPE), polypropylene (PP), polystyrene
(PS), polyvinyl chloride (PVC), makrolon (PC), nylon 6 (PA6), nylon66 fiber (PA66), thermoplastic polyurethane (TPU), ABS
Copolymer, polymethyl methacrylate (PMMA), polyethylene terephthalate (PET), polybutylene terephthalate (PBT)
(PBT), thermoplastic polyimide (TPI), at least one of.
The heat conduction powder of the heat-conductive insulation filling, i.e. melanin covering includes heat conduction powder and its surface coated tool
There is melanin structure thermally conductive insulating layer, it is described that there is melanin structure substance to be covered in the form of being chemically crosslinked with physical absorption
Heat conduction powder surface.
A kind of preparation method of the high heat conductive insulating thermoplastic polymer, including:By the thermoplastic polymer, lead
Thermal insulation filler, processing aid press the weight melt blending, then extrusion molding, granulation.
In the preparation process of Inventive polymers composition, material melts blending temperature is that usual polymer material adds
Blending temperature used in work, can be depending on polymer melting temperature.In addition, according to processing needs, it can be in material be blended
Common some auxiliary agents such as lubricant, antioxidant etc. in polymer processing are added, dosage is conventional amount used, or according to
The requirement of actual conditions is adjusted.
Various batch mixings used in the prior art can be used in the blending equipment of material mixing in the preparation process in accordance with the present invention
Equipment, such as blender, kneader.
Used melt blending equipment is the general blending equipment in Plastics Processing Industry in the preparation process in accordance with the present invention,
Can be double screw extruder, single screw extrusion machine, open mill or mixer etc..
The thermoplastic compounds of the present invention meet good heat conductivility and electrical insulation capability simultaneously, well solve Gao Gong
The work of rate device is encountered thermal conductivity and insulation performance matching problem, can meet current electronic product to heat conductive insulating high score
The performance requirement of sub- material.
Specific implementation mode
With reference to embodiment, further illustrate the present invention.
Embodiment 1:
(1) preparation of poly-dopamine modified metal heat filling Ag powder
0.6 parts by weight Ag powder (upper apron coloured silk Industrial Co., Ltd., spherical shape, 25 μm) is weighed first, and 100 parts by weight are added
In deionized water solution, ultrasound 10min, keeps Ag powder evenly dispersed in ice-water bath;0.05 parts by weight are added in above-mentioned solution
Tyrosine (Aladdin), adjust pH value of solution be 8, then reacted for 24 hours at 45 DEG C;Then centrifugation, washing obtain clean gather
The amine-modified Ag powder of DOPA.
(2) preparation of high heat conductive insulating polypropylene (PP) composite material
By 100 parts by weight of polypropylene (PP) (Zhejiang Xin Chuanjin plastic materials Co., Ltd, the trade mark 3204) resin, poly- DOPA
It is uniform that amine-modified 80 parts by weight of Ag powder heat filling are placed in stirrer for mixing, then adds mixture into double screw extruder
Middle carry out melt blending, extruding pelletization, extrusion temperature are 160~220 DEG C, screw speed 30rpm.By the material grain of extrusion at 90 DEG C
Then dry 12h in baking oven is injected into standard batten under conditions of 160~220 DEG C again, carries out heat conductivility test.
When the content of Ag powder heat-conductive insulation fillings is 80 parts by weight, gained composite material measures body using insulation tester
Product resistivity is 1.7 × 1015Ω cm, it is 6.4Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 2:
(1) preparation of Cu nano wires
2.65 parts by weight Cu (NO3)2(Sinopharm Chemical Reagent Co., Ltd., AR) is dissolved in 800 parts by weight 15mol/L
In NaOH (Sinopharm Chemical Reagent Co., Ltd., AR) solution, 12 parts by weight ethylenediamines are then added, and (Chinese medicines group chemistry tries
Agent Co., Ltd, AR) it is used as end-capping reagent, the hydrazine hydrate (Sinopharm Chemical Reagent Co., Ltd., AR) of 1 parts by weight 35wt% to do
For reducing agent, this mixed process carries out in ice bath.Then by mixed solution at 75 DEG C reaction 1h without mixing.After reaction
Centrifugation is washed up to copper nano-wire.The length of gained copper nano-wire is 10~60 μm, a diameter of 50~400nm.
(2) preparation of poly-dopamine modified metal heat filling Cu nano wires
1 parts by weight Cu copper nano-wires are weighed first to be added in the deionized water solution of 100 parts by weight, it is ultrasonic in ice-water bath
10min keeps Cu nano wires evenly dispersed;The dopamine (Aladdin) of 0.05 parts by weight is added in above-mentioned solution, adjusts solution
PH is 8.5, then reacts 12h at 50 DEG C;Then centrifugation, washing obtain the Cu nano wires of clean poly-dopamine modification.
(3) preparation of high heat conductive insulating polyethylene (PE) composite material
By 100 parts by weight of polyethylene (PE) (Shanghai Su meter Information technologies Co., Ltd, trade mark 5121B) resin, poly- DOPA
It is uniform that amine-modified 30 parts by weight of Cu nano wire heat conductings filler are placed in stirrer for mixing, then adds mixture into twin-screw and squeezes
Go out and carry out melt blending in machine, extruding pelletization, extrusion temperature is 160~220 DEG C, screw speed 30rpm.The material grain of extrusion is existed
Then dry 12h in 90 DEG C of baking ovens is injected into standard batten under conditions of 160~220 DEG C again, carries out heat conductivility test.
When the content of Cu nano wire heat conducting insulating packings is 30 parts by weight, gained composite material is surveyed using insulation tester
It is 3.1 × 10 to obtain volume resistivity15Ω cm, it is 5.2Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 3:
(1) preparation of Ag nanometer sheets
The AgNO of a concentration of 2.35mM of 6 parts by weight3(Sinopharm Chemical Reagent Co., Ltd., AR) aqueous solution and 10 weight
PVP (Sinopharm Chemical Reagent Co., Ltd., the AR) aqueous solutions of part a concentration of 0.2M and a concentration of 4.2mM's of 6 parts by weight
TSC (Sinopharm Chemical Reagent Co., Ltd., AR) aqueous solution is uniformly mixed at room temperature.After stirring 1min, 0.3 is rapidly joined
The NaBH of a concentration of 10mM of parts by weight4(Sinopharm Chemical Reagent Co., Ltd., AR) aqueous solution, the color of solution is by no discoloration
At glassy yellow.Then the silver-colored solution of yellow is put into the single port bottle of 50mL, and is flowed back at 60 DEG C several hours, solution is by Huang
Color gradually becomes blue, shows to have synthesized silver-colored triangular plate.It waits for that sample is cooled to room temperature, obtained sample is centrifuged in 13000rpm
6min, centrifugation gained precipitation are re-dispersed into water.It repeats above-mentioned centrifugal process 3 times, obtains Nano silver piece.Gained Nano silver piece
Length at 1~30 μm, thickness is nanoscale.
(2) preparation of poly-dopamine modification heat filling Ag nanometer sheets
0.1 parts by weight Ag nanometer sheets are weighed first to be added in the deionized water solution of 100 parts by weight, it is ultrasonic in ice-water bath
10min keeps Ag nanometer sheets evenly dispersed;The Dopamine hydrochloride (Aladdin) of 0.02 parts by weight is added in above-mentioned solution, adjusts
PH value of solution is 8.5, then reacts 8h at 60 DEG C;Then centrifugation, washing obtain the Ag nanometer sheets of clean poly-dopamine modification.
(3) preparation of high heat conductive insulating polystyrene (PS) composite material
By 100 parts by weight of polystyrene (PS) (Wenzhou Ou Dengbao Import and Export Co., Ltd.s, the trade mark 635) resin, poly- DOPA
Amine-modified Ag nanometer sheet heat fillings are respectively that be placed in stirrer for mixing uniform for 5,30 parts by weight, are then added mixture into
Melt blending, extruding pelletization are carried out in double screw extruder, extrusion temperature is 160~220 DEG C, screw speed 30rpm.It will squeeze out
Material grain in 90 DEG C of baking ovens dry 12h, be then injected into standard batten under conditions of 160~220 DEG C again, carry out heat conductivility
Test.
When the content of Ag nanometer sheet heat-conductive insulation fillings is 5 parts by weight, gained composite material is surveyed using insulation tester
It is 7.9 × 10 to obtain volume resistivity14Ω cm, it is 1.5Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1.When Ag nanometers
The content of piece heat-conductive insulation filling be 30 parts by weight when, gained composite material use insulation tester measure volume resistivity for
6.4×1015Ω cm, it is 6.5Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 4:
(1) preparation of poly-dopamine modification heat filling Al powder
5 parts by weight Al powder (Hefei Sunrise Aluminium Pigments Co., Ltd., spherical shape, 20 μm, content >=98%) are weighed first to be added
In the deionized water solution of 100 parts by weight, ultrasound 10min, keeps Al powder evenly dispersed in ice-water bath;It is added in above-mentioned solution
The DOPA (Aladdin) of 0.5 parts by weight, it is 10 to adjust pH value of solution, then reacts 5h at 45 DEG C;Then centrifugation, washing are done
The Al powder of net poly-dopamine modification.
(2) preparation of high heat conductive insulating polyvinyl chloride (PVC) composite material
100 parts by weight of polyvinyl chloride (Bo Te polymer performances Materials Co., Ltd of Ningbo City) resin, poly-dopamine are repaiied
It is uniform that 40 parts by weight of Al powder heat filling of decorations are placed in stirrer for mixing, then add mixture into double screw extruder into
Row melt blending, extruding pelletization, extrusion temperature are 160~190 DEG C, screw speed 50rpm.By the material grain of extrusion in 80 DEG C of baking ovens
Then middle dry 12h is injected into standard batten under conditions of 160~190 DEG C again, carry out heat conductivility test.
When the content of Al powder heat-conductive insulation fillings is 40 parts by weight, gained composite material measures body using insulation tester
Product resistivity is 7.2 × 1014Ω cm, it is 1.2Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 5:
(1) preparation of poly-dopamine modification heat filling Zn powder
Weigh first 3 parts by weight Zn powder (Changsha Xin Weilingxin industry Development Co., Ltd, grain size are 15 μm, and the new prestige of the trade mark is insulted,
Zn content >=96%, spherical) be added in the deionized water solution of 100 parts by weight, ultrasound 10min, keeps Zn powder equal in ice-water bath
Even dispersion;The tyrosine (Aladdin) of 1.5 parts by weight is added in above-mentioned solution, it is 9 to adjust pH value of solution, then anti-at 55 DEG C
Answer 16h;Then centrifugation, washing obtain the Zn powder of clean poly-dopamine modification.
(2) preparation of high heat conductive insulating polymethyl methacrylate (PMMA) composite material
For polymethyl methacrylate (PMMA) (Dongguan City Di Ke plastic materials Co., Ltd, trade mark MH) resin:It will
100 parts by weight of plexiglass, 60 parts by weight of Zn powder heat filling of poly-dopamine modification are placed in blender
Be uniformly mixed, then add mixture into and carry out melt blending in double screw extruder, extruding pelletization, extrusion temperature be 190~
270 DEG C, screw speed 50rpm.By the material grain of extrusion in 90 DEG C of baking ovens dry 12h, then again under conditions of 190~270 DEG C
It is injected into standard batten, carries out heat conductivility test.
When the content of Zn powder heat-conductive insulation fillings is 60 parts by weight, gained composite material measures body using insulation tester
Product resistivity is 5.2 × 1014Ω cm, it is 1.4Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 6:
(1) preparation of poly-dopamine modification heat filling Cu powder
Weighing 2 parts by weight Cu powder first, (Nangong City Plain alloy material Co., Ltd, grain size are 300nm~25 μm, the trade mark
Plain, copper content >=99% are spherical) it is added in the deionized water solution of 100 parts by weight, ultrasound 10min, makes Cu in ice-water bath
Powder is evenly dispersed;The dopamine (Aladdin) of 1.6 parts by weight is added in above-mentioned solution, it is 8.5 to adjust pH value of solution, then 70
10h is reacted at DEG C;Then centrifugation, washing obtain the Cu powder of clean poly-dopamine modification.
(2) preparation of high heat conductive insulating high density polyethylene (HDPE) (HDPE) composite material
By 100 weight of high density polyethylene (HDPE) (HDPE) (Yuyao City steps more plasticizing Co., Ltds, trade mark DMDA-8008) resin
Part, that 70 parts by weight of Cu powder heat filling of poly-dopamine modification are placed in stirrer for mixing is uniform, then add mixture into double
Melt blending, extruding pelletization are carried out in screw extruder, extrusion temperature is 160~220 DEG C, screw speed 30rpm.By extrusion
Expect grain dry 12h in 90 DEG C of baking ovens, is then injected into standard batten under conditions of 160~220 DEG C again, carries out heat conductivility survey
Examination.
When the content of Cu powder heat-conductive insulation fillings is 70 parts by weight, it is 4.6 × 10 to obtain volume resistivity15Ω cm, heat
It is 5.3Wm that conductance tester, which measures thermal coefficient,-1·K-1。
Embodiment 7:
(1) preparation of Ag nano wires
A, 4 parts by weight ethylene glycol (Sinopharm Chemical Reagent Co., Ltd., AR) are first added, heat 10min, then with note
2 parts by weight silver nitrate (AgNO are added in emitter3) (Sinopharm Chemical Reagent Co., Ltd., AR) ethylene glycol solution (2 × 10- 4M), 15min is reacted.
B, 10 parts by weight AgNO are rapidly joined into three-necked bottle with syringe3Ethylene glycol solution (0.1M), then slowly
The ethylene glycol solution of (control is in 10min or so) 20 parts by weight PVP (Sinopharm Chemical Reagent Co., Ltd., GR) is added
(0.3M is obtained by the repetitive unit molar amount of PVP) then proceedes to reaction 2h.Centrifugation alcohol is washed to get silver nanoparticle after reaction
Line.The length of gained nano silver wire is at 20~40 μm, and diameter is in 60~200nm.
(2) preparation of poly-dopamine modification heat filling Ag nano wires
0.5 parts by weight Ag nano wires are weighed first to be added in the deionized water solution of 100 parts by weight, it is ultrasonic in ice-water bath
10min keeps Ag nano wires evenly dispersed;The DOPA (Aladdin) of 0.5 parts by weight is added in above-mentioned solution, adjusting pH value of solution is
8.5, then 18h is reacted at 70 DEG C;Then centrifugation, washing obtain the Ag nano wires of clean poly-dopamine modification.
(3) preparation of high heat conductive insulating ABS resin composite material
100 parts by weight of ABS (Ju Tai engineering plastics Co., Ltd of city of Kunshan, trade mark PA-747) resin, poly-dopamine are repaiied
It is uniform that 20 parts by weight of Ag nano wire heat conductings filler of decorations are placed in stirrer for mixing, then adds mixture into double screw extruder
Middle carry out melt blending, extruding pelletization, extrusion temperature are 190~235 DEG C, screw speed 40rpm.By the material grain of extrusion at 80 DEG C
Then dry 12h in baking oven is injected into standard batten under conditions of 190~235 DEG C again, carries out heat conductivility test.
When the content of Ag nano wire heat conducting insulating packings is 20 parts by weight, gained high heat conductive insulating ABS resin composite wood
Material uses insulation tester to measure volume resistivity as 2.5 × 1014Ω cm, Conduction Coefficient Detector Basing measure thermal coefficient and are
5.3W·m-1·K-1。
Embodiment 8:
(1) preparation of poly-dopamine modification heat filling multi-walled carbon nanotube
1.5 parts by weight multi-walled carbon nanotube (Timestub are weighed firstTMHigh-purity multi-walled carbon nanotube, the Chinese Academy of Sciences at
All organic chemistry Co., Ltd produces, purity >=90wt%, overall diameter >=50nm, and length is 10~30 μm) 100 parts by weight are added
Deionized water solution in, ultrasound 10min, keeps carbon nanotube evenly dispersed in ice-water bath;3 weight are added in above-mentioned solution
The dopamine (Aladdin) of part, it is 9 to adjust pH value of solution, is then reacted for 24 hours at 50 DEG C;Subsequent centrifugation, washing obtain clean
The carbon nanotube of poly-dopamine modification.
2) preparation of high heat conductive insulating nylon -66 (PA-66) composite material
100 parts by weight of nylon66 fiber (Dongguan City tortoise beetle plastic cement Co., Ltd, trade mark A3WG10) resin, poly-dopamine are modified
10 parts by weight of multi-walled carbon nanotube heat filling to be placed in stirrer for mixing uniform, then add mixture into twin-screw extrusion
Melt blending, extruding pelletization are carried out in machine, extrusion temperature is 250~290 DEG C, screw speed 70rpm.By the material grain of extrusion 95
Then dry 12h in DEG C baking oven is injected into standard batten under conditions of 250~290 DEG C again, carries out heat conductivility test.
When the content of multi-walled carbon nanotube heat-conductive insulation filling is 10 parts by weight, gained composite material uses Insulation test
It is 7.3 × 10 that instrument, which measures volume resistivity,13Ω cm, it is 4.0Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 9:
(1) preparation of poly-dopamine modification heat filling graphene
4 parts by weight of graphite alkene (TimsGraph are weighed firstTMGraphene, the limited public affairs of Chinese Academy of Sciences's Chengdu organic chemistry
Department's production, purity >=95wt%, a diameter of 0.5~3 μm, the number of plies is 1~10 layer, and thickness is 0.55~3.74nm) 100 weights are added
In the aqueous solution for measuring part, ultrasound 10min, makes graphene uniform disperse in ice-water bath;4.8 parts by weight are added in above-mentioned solution
Dopamine hydrochloride (Aladdin), adjust pH value of solution be 9.5, then react 14h at 55 DEG C;Then centrifugation, washing are done
The graphene of net poly-dopamine modification.
(2) preparation of high heat conductive insulating thermoplastic polyurethane (TPU) composite material
By 100 parts by weight of thermoplastic polyurethane (Dongguan City Xin Yu plastic cement Co., Ltd, trade mark R195A-9TPU) resin, gather
The amine-modified heat filling of DOPA is respectively that be placed in stirrer for mixing uniform for 10,20 parts by weight, is then added mixture into double
Melt blending, extruding pelletization are carried out in screw extruder, extrusion temperature is 180~220 DEG C, screw speed 60rpm.By extrusion
Expect grain dry 12h in 80 DEG C of baking ovens, is then injected into standard batten under conditions of 180~220 DEG C again, carries out heat conductivility survey
Examination.
When the content of graphene heat-conductive insulation filling is 10 parts by weight, gained composite material is measured using insulation tester
Volume resistivity is 1.8 × 1014Ω cm, it is 3.2Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1.When graphene is led
When the content of thermal insulation filler is 20 parts by weight, gained composite material use insulation tester measure volume resistivity for 6.9 ×
1016Ω cm, it is 6.1Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 10:
(1) preparation of poly-dopamine modification heat filling carbon fiber
1 parts by weight of carbon fibers (C-25 carbon nano-fibers, Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences's life are weighed first
Production, purity 99wt%, fibre diameter:150-200nm, length:10~20 microns) it is added in the aqueous solution of 100 parts by weight, in ice
Ultrasound 10min, keeps carbon fiber evenly dispersed in water-bath;Dopamine hydrochloride (I of 1.6 parts by weight is added in above-mentioned solution
Fourth), it is 8 to adjust pH value of solution, then reacts 12h at 60 DEG C;Then centrifugation, washing obtain the carbon of clean poly-dopamine modification
Fiber.
(2) preparation of high heat conductive insulating PP composite material
By acrylic resin (Zhejiang Xin Chuanjin plastic materials Co., Ltd, the trade mark 3204) 100 parts by weight, poly-dopamine is repaiied
To be placed in stirrer for mixing uniform for 30 parts by weight respectively for the carbon fiber heat filling of decorations, then adds mixture into twin-screw extrusion
Melt blending, extruding pelletization are carried out in machine, extrusion temperature is 160~220 DEG C, screw speed 30rpm.By the material grain of extrusion 90
Then dry 12h in DEG C baking oven is injected into standard batten under conditions of 160~220 DEG C again, carries out heat conductivility test.
When the content of carbon fiber heat-conductive insulation filling is 30 parts by weight, gained composite material is measured using insulation tester
Volume resistivity is 5.7 × 1014Ω cm, it is 7.1Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Embodiment 11:
(1) preparation of poly-dopamine modification heat filling single-walled carbon nanotube
2 parts by weight multi-walled carbon nanotube (Timsstub are weighed firstTMHigh-purity single-walled carbon nanotube, Chinese Academy of Sciences Chengdu
Organic chemistry Co., Ltd produces, purity >=90wt%, and overall diameter is 1~2nm, and length is 5~30 μm) 100 parts by weight are added
Aqueous solution in, ultrasound 10min, keeps carbon nanotube evenly dispersed in ice-water bath;1.2 parts by weight are added in above-mentioned solution
DOPA (Aladdin), it is 10 to adjust pH value of solution, then reacts 5h at 60 DEG C;Then centrifugation, washing obtain clean poly- DOPA
Amine-modified carbon nanotube.
(2) preparation of high heat conductive insulating composite polyethylene material
By 100 parts by weight of polyethylene (PE) (Shanghai Su meter Information technologies Co., Ltd, trade mark 5121B) resin, poly- DOPA
It is uniform that amine-modified 15 parts by weight of single-walled carbon nanotube heat filling are placed in stirrer for mixing, then adds mixture into double spiral shells
Melt blending, extruding pelletization are carried out in bar extruder, extrusion temperature is 160~220 DEG C, screw speed 30rpm.By the material of extrusion
Then grain dry 12h in 90 DEG C of baking ovens is injected into standard batten under conditions of 160~220 DEG C again, carries out heat conductivility survey
Examination.
When the content of single-walled carbon nanotube heat-conductive insulation filling is 15 parts by weight, gained composite material uses Insulation test
It is 1.3 × 10 that instrument, which measures volume resistivity,12Ω cm, it is 3.7Wm that Conduction Coefficient Detector Basing, which measures thermal coefficient,-1·K-1。
Comparative example 1:
It is not added with any heat filling, acrylic resin is molded extruding pelletization according to common process, measures polyacrylic lead
Hot coefficient is 0.22Wm-1·K-1, volume resistivity is 2.8 × 1015Ω·cm。
Comparative example 2:
The acrylic resin of 80 parts by weight of silver powder modified without poly-dopamine and 100 parts by weight is placed in blender and is mixed
It closes uniformly, extruding pelletization is molded according to common process.The thermal coefficient for measuring composite material is 6.1Wm-1·K-1, volume electricity
Resistance rate is 4.4 × 103Ω·cm。
Comparative example 1 and comparison ratio 2, after the silver powder without poly-dopamine modification is added in polypropylene, composite material
Thermal coefficient has significant raising, heat conductivility to significantly improve.But the volume resistivity of composite material significantly reduces, it is conductive
Ability is enhanced, on-insulated so as to cause composite material;
Compared with embodiments herein 1:" when the content of Ag powder heat-conductive insulation fillings is 80 parts by weight, gained is compound
Material uses insulation tester to measure volume resistivity as 1.7 × 1015Ω cm, Conduction Coefficient Detector Basing measure thermal coefficient and are
6.4W·m-1·K-1", after the silver powder after poly-dopamine is modified is added in acrylic resin, the thermal coefficient of composite material
Do not have a greater change, still, resistivity is substantially increased, thus can be illustrated, under the premise of not influencing thermal conductivity of material,
After silver powder after poly-dopamine is modified is added to acrylic resin, the conductive path between silver powder is cut off, to drop
The low electric conductivity of material, compound material insulation.
In conclusion system is blended with thermoplastic polymer as filler using the heat conduction powder of poly-dopamine modification by the present invention
Standby composite material has higher thermal conductivity, while material still keeps good electrical insulating property.
Example above-mentioned is merely illustrative, some features of feature for explaining the present invention.The attached claims
It is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation, not to the limitation in any form done of the present invention, therefore all do not fall off this hair
The content of bright technical solution, according to the technical essence of the invention to above example make it is any it is simple modification, equivalent variations with
Modification, in the range of still falling within technical solution of the present invention.
Claims (9)
1. a kind of high heat conductive insulating thermoplastic polymer, it is characterised in that the thermoplastic polymer is by including following components
Raw material is blended and obtains:
Each component is counted in parts by weight,
100 parts by weight of thermoplastic resin;
5~80 parts by weight of heat-conductive insulation filling;
The heat-conductive insulation filling is heat conduction powder and its is surface coated with melanin structure thermally conductive insulating layer;
The heat conduction powder is metal simple-substance or carbon-based powder;
It is described that have melanin structure thermally conductive insulating layer be metal heat-conducting powder by DOPA, dopamine, Dopamine hydrochloride, tyrosine
At least one of substance by surface be modified gained.
2. high heat conductive insulating thermoplastic polymer as described in claim 1, it is characterised in that:
The metal simple-substance is Au, Ag, Cu, Mg, Al, Fe, Ni, Be, Ca, Pt or Zn;
The carbon-based powder is graphite, carbon fiber, carbon nanotube, fullerene, graphene or amorphous carbon;
The shape of the heat conduction powder includes granular, sheet, spherical shape or threadiness.
3. high heat conductive insulating thermoplastic polymer as claimed in claim 2, it is characterised in that:
A diameter of 20~500nm of linear heat conduction powder, length are 10~120 μm, and draw ratio is between 100~1000;
Spherical or granular heat conduction powder diameter is in 10nm~50 μm;
For sheet heat conduction powder length in 200nm~100 μm, thickness is nanoscale.
4. high heat conductive insulating thermoplastic polymer as described in claim 1, it is characterised in that the heat-conductive insulation filling be by
Method comprising the following steps are prepared:
A. heat conduction powder dispersion liquid is prepared;
B. at least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance are added into heat conduction powder dispersion liquid,
The heat-conductive insulation filling is made in polymerization.
5. high heat conductive insulating thermoplastic polymer as claimed in claim 4, it is characterised in that:
In step a, deionized water and heat conduction powder amount ratio are 1 in heat conduction powder dispersion liquid:(0.001~0.05);
In step b, heat conduction powder and the amount ratio of at least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance are
1:(0.05~2).
6. high heat conductive insulating thermoplastic polymer as claimed in claim 5, it is characterised in that the heat-conductive insulation filling be by
Method comprising the following steps are prepared:
Ultrasonic disperse is added in deionized water to uniformly obtaining metal heat-conducting powder dispersion liquid in heat conduction powder by a;
At least one of DOPA, dopamine, Dopamine hydrochloride, tyrosine substance is added in b in above-mentioned solution, adjusts solution ph
It is 8~10, react 5 at 45 DEG C~70 DEG C~for 24 hours, and it is dry after washing after reaction through centrifugation, the heat conductive insulating is made
Powder.
7. high heat conductive insulating thermoplastic polymer as described in claim 1, it is characterised in that:
The thermoplastic resin is polyethylene, high density polyethylene (HDPE), polypropylene, polystyrene, polyvinyl chloride, makrolon, Buddhist nun
Dragon 6, nylon66 fiber, thermoplastic polyurethane, Acrylonitrile Butadiene-Styrene copolymer, polymethyl methacrylate, polyethylene terephthalate, poly- pair
At least one of benzene dicarboxylic acid butanediol ester, thermoplastic polyimide.
8. high heat conductive insulating thermoplastic polymer as described in claim 1, it is characterised in that:
The thermoplastic resin is 100 parts by weight meters, and the graininess heat filling is 40~80 parts by weight, linear heat filling
For 5~30 parts by weight, sheet heat filling is 5~30 parts by weight.
9. a kind of preparation method of high heat conductive insulating thermoplastic polymer as described in one of claim 1~8, it is characterised in that
The method includes:
The high heat conductive insulating thermoplastic polymer is made after pressing the dosage melt blending in the component.
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