CN109679142A - Preparation method of composite heat-conducting filler for high polymer - Google Patents
Preparation method of composite heat-conducting filler for high polymer Download PDFInfo
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- CN109679142A CN109679142A CN201811540335.7A CN201811540335A CN109679142A CN 109679142 A CN109679142 A CN 109679142A CN 201811540335 A CN201811540335 A CN 201811540335A CN 109679142 A CN109679142 A CN 109679142A
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- 239000000945 filler Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 229920000642 polymer Polymers 0.000 title abstract description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 6
- 230000009471 action Effects 0.000 claims abstract description 3
- 239000011812 mixed powder Substances 0.000 claims abstract description 3
- 238000011049 filling Methods 0.000 claims description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 229920002521 macromolecule Polymers 0.000 claims description 10
- 229910052582 BN Inorganic materials 0.000 claims description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 8
- 229910017083 AlN Inorganic materials 0.000 claims description 7
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- -1 magnesium nitride Chemical class 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 239000003575 carbonaceous material Substances 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 230000001588 bifunctional effect Effects 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000011231 conductive filler Substances 0.000 claims 1
- 229910021389 graphene Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000007385 chemical modification Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000989 Alclad Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000004756 silanes Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a preparation method of a composite heat-conducting filler for polymers, which comprises the steps of firstly, uniformly mixing at least two heat-conducting fillers in proportion, then placing mixed solid at the bottom of a centrifugal tube, and then placing aqueous solution of a silane coupling agent on the upper part of mixed powder; or firstly placing the aqueous solution of the silane coupling agent at the bottom of a centrifugal tube, and then placing the mixed solid on the upper part of the aqueous solution; and then, uniformly mixing the two materials under the centrifugal action of a centrifugal machine, and finally drying and ball-milling to obtain the composite heat-conducting filler for the polymer. The invention utilizes the centrifugal force of the centrifuge to quickly complete the chemical modification of the silane coupling agent and the filler, and improves the interface combination between the filler and between the filler and the matrix, thereby being beneficial to the formation of a heat conduction network and improving the heat conductivity. The method has short operation time and simple process, and can be used for industrial production.
Description
Technical field:
The present invention relates to a kind of preparation method of heat filling more particularly to a kind of compound heat fillings of macromolecule
Preparation method.
Background technique:
The thermal conductivity of high molecular material itself is relatively low, and the filler with heating conduction is distributed to group in polymeric matrix
At heat-conductive composite material be major way that current heat-conducting plastic uses.Heat filling mainly includes nitride, oxide, carbon
Compound and carbon material etc..However filler can reduce technical effect in the interface cohesion difference of matrix and excessively high filling proportion,
And higher cost, to limit its scope of application.Therefore people develop various technological means and improve answering for fillers and polymer
Efficiency is closed, composite cost is simplified, improves polymer thermal conductivity.It is such as compounded by big small particle and increases packing density, mutually filled up
Gap forms intensive thermal conducting path.Or be used in compounding different heat fillings in thermally conductive system, thus the macromolecule that extends
The use scope of material.
Such as Chinese patent (CN201810238974) heat filling is the boron nitride particle comprising particle size not
It with the mixture of aluminum nitride particle, is scattered in matrix with specific mixing ratio, due to the boron nitride particle and aluminium nitride
Synergistic effect between grain obtains and possesses when they are used alone the composite material of more high-termal conductivity.Chinese patent
(CN200910192629) carbon alclad nanoparticle is added in silane coupling agent alcoholic solution and is stirred, dry 10h at 120 DEG C,
Then 1h is dried at 150 DEG C, obtained carbon modified alclad nanoparticle, but this method agitating mode is single.Chinese patent (Shen
Please number: CN201510957195) only with physical mixed, by metal oxide, nitride and polyester fiber in 60-80r/min
Stirring rate under be blended doping, squeezed out using double screw extruder, the two obviously lacks stable bond.Chinese patent (application
Number: a kind of thermally conductive wear resistant filler CN201410007202) is prepared, carbon nanotube and cubic boron nitride are mixed through high-speed mixer
It closes, then is dipped in progress ultrasonic disperse processing in dehydrated alcohol, last ball milling, freeze-drying, grinding are sintered at a temperature of 1560 DEG C
To obtain the final product.Chinese patent (application number: CN201510873371) carries out pre-treatment to inorganic filler, is by inorganic filler powder and water
After alcohol mixing, ultrasonic agitation is uniform, then inorganic filler suspension is added in silane coupling agent, and stirring is separated by solid-liquid separation, washing, does
It is dry, so that inorganic filler surface is completely covered in polar silanes group, obtain a kind of high heat conductivity insulation composite, these types of technique
It is all relatively cumbersome.There are also Chinese patents (application number: CN201610249893) by nanofiller high-speed emulsifying machine, high-speed stirred
Instrument or Ultrasonic Cell Disruptor are scattered in aqueous surfactant solution, are then added in aqueous high molecular lotion, are obtained multiple emulsion,
It is demulsified by the way of adding electrolyte, after filtering and water removal, nanometer is pressed by hot pressing or extrusion process and fiber cloth
Filler modified prepreg or nano-filler modified composite material.
Summary of the invention:
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of macromolecule systems of compound heat filling
Preparation Method can make polymer have high thermal conductivity coefficient after the composite heat-conducting filler that preparation is added.
Technical solution provided by the invention is as follows: a kind of preparation method of macromolecule with compound heat filling, feature
Be, first mix in proportion at least two heat fillings, after hybrid solid object is placed in centrifugation bottom of the tube, then by silane
The aqueous solution of coupling agent is placed in mixed powder top；Or the aqueous solution of silane coupling agent is first placed in centrifugation bottom of the tube, then will mix
It closes solids and is placed in aqueous solution top；Then the two is uniformly mixed by the centrifugal action of centrifuge, finally by drying, ball
It grinds to get the compound heat filling of macromolecule is arrived.
It is preferred that above-mentioned heat filling is nitride, oxide, carbide or carbon material etc..More preferable above-mentioned heat filling is
For boron nitride, aluminium nitride, magnesium nitride, magnesia, aluminium oxide, zinc oxide, silicon carbide, carbon fiber, graphite, carbon nanotube or graphite
Alkene etc..
It is preferred that above-mentioned silane coupling agent is at least one of bifunctional silane coupling agent, specially double-(2- (three second
Oxysilane) propyl)-tetrasulfide or double-(γ-(triethoxysilicane) propyl)-disulphide etc..
It is preferred that above-mentioned composite heat-conducting filler at least contains two different heat fillings；Wherein thermal conductivity filler quality content is most
It is less 1%, up to 99%.
It is preferred that above-mentioned silane coupling agent concentration of aqueous solution is 20%~50%；The silane coupling agent amount of aqueous solution used is to lead
The 10%-100% of hot packing quality.
It is preferred that above-mentioned centrifuge speed is 2000-15000rpm, centrifugation time 1-20min；The drying temperature is 40-
80℃；The rotational speed of ball-mill is 70-670r/min, and (at room temperature) Ball-milling Time is 12-24h.
The utility model has the advantages that
The centrifugal force that the present invention is generated by centrifuge is quickly mixed several heat fillings and silane coupling agent, and
Promote hydrolysis using the heat that centrifugation shearing generates, generates different heat fillings directly quickly and effectively combine.With
Passing technology is compared, it is clear that the features such as having modification time fast, do not generate a large amount of waste water, be suitble to industrialization.
Specific embodiment:
The specific implementation case that a kind of macromolecule is chosen with compound heat filling and preparation method thereof according to the present invention
Under such as:
Embodiment 1:
By 5g boron nitride, 5g aluminium nitride is uniformly mixed by ball mill, dry to be placed on centrifugation bottom of the tube, and 1g is added in top
The aqueous solution of double-(2- (triethoxysilane) propyl)-tetrasulfide, aqueous solution mass concentration are 20%, are placed in a centrifuge
It is centrifuged 1 minute under revolving speed 2000rpm again, dry ball milling after taking-up, drying temperature is 60 DEG C, rotational speed of ball-mill 400r/min, ball
15h consume time to get corresponding macromolecule composite heat-conducting filler is arrived.Composite heat-conducting filler is mixed into hot-forming test with PBT
Thermal conductivity, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), and thermal conductivity is 1.6W/ after the heat filling of preparation is added
(m.K), the results showed that prepared heat filling is a kind of compounded mix that can effectively improve PBT thermal conductivity.
Embodiment 2
Silane coupling agent is double-(γ-(triethoxysilicane) propyl)-curing to the present embodiment unlike the first embodiment
Object, using the centrifuge speed of 7000rpm, centrifugation time 20min, dry ball milling after taking-up, drying temperature is 40 DEG C, ball milling
Revolving speed is 100r/min, Ball-milling Time 20h, other same as Example 1.Composite heat-conducting filler is mixed with PBT hot-forming
Test thermal conductivity, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), and thermal conductivity is after the heat filling of preparation is added
1.62W/ (m.K), the results showed that prepared heat filling is a kind of compounded mix that can effectively improve PBT thermal conductivity.
Embodiment 3
The present embodiment use unlike the first embodiment 5g it is bis--water of (2- (triethoxysilane) propyl)-tetrasulfide
Solution, aqueous solution mass concentration are 50%, and using the centrifuge speed of 15000rpm, centrifugation time 10min is dry after taking-up
Ball milling, drying temperature is 80 DEG C, rotational speed of ball-mill 600r/min, Ball-milling Time 12h, other same as Example 1.By composite guide
Hot filler mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), and preparation is added
Heat filling after thermal conductivity be 1.58W/ (m.K), the results showed that prepared heat filling be one kind can effectively improve PBT
The compounded mix of thermal conductivity.
Embodiment 4
The present embodiment uses 0.1g boron nitride, 9.9g graphite unlike the first embodiment, other same as Example 1.It will
Composite heat-conducting filler mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), is added
Thermal conductivity is 1.23W/ (m.K) after entering the heat filling of preparation, the results showed that prepared heat filling is that one kind can be effective
Improve the compounded mix of PBT thermal conductivity.
Embodiment 5
The present embodiment uses 9.9g boron nitride, 0.1g graphite unlike the first embodiment, other same as Example 1.It is multiple
It closes heat filling and mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), is added
Thermal conductivity is 1.30W/ (m.K) after the heat filling of preparation, the results showed that prepared heat filling is that one kind can be mentioned effectively
The compounded mix of high PBT thermal conductivity.
Embodiment 6
The present embodiment uses 5g magnesia, 5g silicon carbide unlike the first embodiment, other same as Example 1.It is compound
Heat filling mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), and system is added
Thermal conductivity is 1.13W/ (m.K) after standby heat filling, the results showed that prepared heat filling can effectively improve for one kind
The compounded mix of PBT thermal conductivity.
Embodiment 7
The present embodiment uses 5g aluminium nitride, 5g silicon carbide unlike the first embodiment, other same as Example 1.It is compound
Heat filling mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is 0.27W/ (m.K), and system is added
Thermal conductivity is 0.948W/ (m.K) after standby heat filling, the results showed that prepared heat filling can effectively improve for one kind
The compounded mix of PBT thermal conductivity.
Embodiment 8
The present embodiment uses 0.1g aluminium nitride, 0.1g carbon nanotube unlike the first embodiment, and 9.8g silicon carbide is other
It is same as Example 1.Composite heat-conducting filler mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is
0.27W/ (m.K), thermal conductivity is 0.758W/ (m.K) after the heat filling of preparation is added, the results showed that prepared heat filling
For a kind of compounded mix that can effectively improve PBT thermal conductivity.
Embodiment 9
The present embodiment uses 3.3g aluminium nitride, 3.4g carbon nanotube unlike the first embodiment, and 3.3g silicon carbide is other
It is same as Example 1.Composite heat-conducting filler mixes hot-forming test thermal conductivity with PBT, the results showed that, pure PBT thermal conductivity is
0.27W/ (m.K), thermal conductivity is 1.32W/ (m.K) after the heat filling of preparation is added, the results showed that prepared heat filling
For a kind of compounded mix that can effectively improve PBT thermal conductivity.
Claims (7)
1. a kind of macromolecule preparation method of compound heat filling, which is characterized in that first press at least two heat fillings
Ratio is uniformly mixed, after hybrid solid object is placed in centrifugation bottom of the tube, then the aqueous solution of silane coupling agent is placed in mixed powder
Top；Or the aqueous solution of silane coupling agent is first placed in centrifugation bottom of the tube, then hybrid solid object is placed in aqueous solution top；Then
The two is uniformly mixed by the centrifugal action of centrifuge, finally by drying, ball milling to get to macromolecule with compound thermally conductive
Filler.
2. according to preparation method described in right 1, it is characterised in that the heat filling be nitride, oxide, carbide or
Carbon material.
3. according to preparation method described in right 1, it is characterised in that the heat filling be boron nitride, aluminium nitride, magnesium nitride,
Magnesia, aluminium oxide, zinc oxide, silicon carbide, carbon fiber, graphite, carbon nanotube or graphene.
4. according to preparation method described in right 1, it is characterised in that the silane coupling agent is in bifunctional silane coupling agent
At least one, specially double-(2- (triethoxysilane) propyl)-tetrasulfide or double-(γ-(triethoxysilicane) third
Base)-disulphide.
5. according to preparation method described in right 1, it is characterised in that the composite heat-conducting filler at least contains two different lead
Hot filler；Wherein thermal conductivity filler quality content is at least 1%, up to 99%.
6. according to preparation method described in right 1, it is characterised in that the silane coupling agent concentration of aqueous solution is 20%~50%；
The silane coupling agent amount of aqueous solution used is the 10%-100% of thermal conductivity filler quality.
7. according to preparation method described in right 1, it is characterised in that the centrifuge speed is 2000-15000rpm, when centrifugation
Between be 1-20min；The drying temperature is 40-80 DEG C；The rotational speed of ball-mill is 70-670r/min, Ball-milling Time 12-24h.
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| CN201811540335.7A CN109679142A (en) | 2018-12-17 | 2018-12-17 | Preparation method of composite heat-conducting filler for high polymer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138832A (en) * | 2019-12-16 | 2020-05-12 | 湖南文理学院 | Method for preparing BN thermal interface material |
| CN112063301A (en) * | 2020-07-31 | 2020-12-11 | 新昌县易纵新材料科技有限公司 | High-strength heat-conducting modified epoxy resin composite coating and preparation method thereof |
| CN113637338A (en) * | 2021-08-18 | 2021-11-12 | 天津大学 | Modified hexagonal boron nitride, water-based anti-oxidation anticorrosive coating and preparation method thereof |
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Effective date of registration: 20190722 Address after: 215626 No. 1 Xingyu West Road, Hexing, Jinfeng Town, Zhangjiagang City, Suzhou City, Jiangsu Province Applicant after: JIANGSU BOLIN PLASTICS Co.,Ltd. Applicant after: Nanjing Tech University Address before: 210009 Gulou District, Jiangsu, Nanjing new model road, No. 5 Applicant before: Nanjing Tech University |
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