CN101283049A - Thermally conductive resin composition - Google Patents
Thermally conductive resin composition Download PDFInfo
- Publication number
- CN101283049A CN101283049A CNA2006800378220A CN200680037822A CN101283049A CN 101283049 A CN101283049 A CN 101283049A CN A2006800378220 A CNA2006800378220 A CN A2006800378220A CN 200680037822 A CN200680037822 A CN 200680037822A CN 101283049 A CN101283049 A CN 101283049A
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- Prior art keywords
- resin composition
- conductive resin
- resin
- magnesite
- polyarylene sulfide
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
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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)
Abstract
Disclosed is a material having a high thermal conductivity, which is excellent in moldability, wet heat resistance and wear characteristics. Specifically, 50-500 parts by weight of a magnesite containing no crystal water is blended per 100 parts by weight of a polyarylene sulfide resin.
Description
Technical field
The present invention relates to injection molding, extrusion moulding is good, humidity resistance and wearing character good, the heat conductance resin combination.
Background technology
With polyphenylene sulfide (below be abbreviated as PPS) resin is poly (arylene sulfide) (below the be abbreviated as PAS) resin of representative, because have high thermotolerance, mechanical properties, chemical proofing, dimensional stability, flame retardant resistance, and be widely used in electrical equipment, e-machine component materials, automobile machine part material, the chemical machine part material etc.In recent years, there is the problem of heat release in frivolous, short and smallization of these parts in the inside of parts etc., requiring to provide the material of exothermicity.
Based on such reason, proposed in the PPS resin, to add the aluminum oxide of specified particle diameter, improve the method (JP-A 2002-146187) of formability and thermal conductivity, though improved formability in this method, but because the Mohs' hardness height of aluminum oxide, when or moulding mixing with resin, the screw rod of forcing machine, shaper, barrel or shaping mould wear and tear tempestuously, have the problem of tramp m..
On the other hand, proposed in the PPS resin, to cooperate graphite, give the method (JP-A 2003-41119) of its thermal conductivity, though can not cause the wear problems such as screw rod that cause by filler in this method, but owing to provide thermal conductivity and electroconductibility, the problem that existence can not be used simultaneously in requiring the field of electrical insulating property.
Therefore, proposed to add as resin the thermal conductivity filler of usefulness, when adopting insulativity, thermal conductivity is higher, and the low magnesium oxide of Mohs' hardness ratio aluminum oxide, and in order to improve wet fastness, covers its surperficial filler (JP-A 2003-34523) with silicon-dioxide.But, when using this filler, though wet fastness has at normal temperatures improved, but the temperature tolerance (humidity resistance) under hot and humid is poor, in the such test of pressure cooking test (below abbreviate PCT as), exist magnesium oxide to become magnesium hydroxide, resin albefaction, expansion, the significantly reduced problem of mechanical properties.
Summary of the invention
The object of the present invention is to provide formability, humidity resistance and wearing character material good, that thermal conductivity is high.
The inventor found that with respect to pas resin through wholwe-hearted research, by cooperating the magnesite that does not contain crystal water, can improve formability, humidity resistance and wearing character, thereby finish the present invention.
That is, the present invention is a kind of heat conductive resin composition, and it is with respect to the polyarylene sulfide resin of 100 weight parts, cooperate 50～500 weight parts do not contain crystal water, by chemical formula MgCO
3Shown magnesite forms.
Embodiment
Explain the present invention below.The pas resin of using among the present invention is with the main resin that constitutes of repeating unit-(Ar-S)-(Ar is an arylidene) serve as.As arylidene, for example can use to phenylene, metaphenylene, adjacent phenylene, the phenylene of replacement, p p '-diphenylene sulfuryl, p, p '-biphenylene, p, p '-diphenylene ether, p, p '-diphenylene carbonyl, naphthylidene etc.At this moment, in the arylene sulfide ether that constitutes by above-mentioned arylidene, except the polymkeric substance that uses identical repeating unit is homopolymer, consider, preferably comprise different multipolymers of planting repeating units from the processibility of composition.
As homopolymer, preferred especially use as arylidene use to phenylene, repeating unit is the product to the poly (phenylene sulfide) ether group.And, as multipolymer, contain in the arylene sulfide ether of above-mentioned arylidene, can use the different combinations more than two kinds, wherein preferred especially use comprises the combination to poly (phenylene sulfide) ether and metaphenylene thioether group.Wherein, contain 70 moles of % above to the poly (phenylene sulfide) ether, it is above preferably to contain 80 moles of %, considers to be fit to from rerum naturas such as thermotolerance, flowability (formability), mechanical characteristicies.
And, in these pas resins, especially preferably use the high-molecular weight polymer that is essentially straight chain structure that obtains through polycondensation as the monomer of main body with two functionality halogenated aromatic compounds, except the pas resin of straight chain structure, use the monomers such as many halogenated aromatic compounds that have the halogenic substituent more than three on a small quantity during condensation, also can use part to form the polymkeric substance of branched structure or crosslinking structure, also can use in the presence of oxygen or oxygenant, make the oxidation cross-linked or heat cross-linking raising melt viscosity of polymkeric substance of the straight chain structure of lower molecular weight by heat, the polymkeric substance of improvement processing forming or their mixture.
And the pas resin that uses among the present invention is that (310 ℃ of down cut speed are 1000sec with above-mentioned straight chain shape pas resin
-1Under viscosity be 10～300Pas) for main body, its part (1～30 weight % is preferably 2～25 weight %) is that higher (300～3000Pas, preferred 500～2000Pas) the branching or the mixed stocker of crosslinked pas resin are also passable with viscosity.And the pas resin that uses among the present invention preferably carries out acid elution, hot wash, organic solvent washing (or their combination) etc. after polymerization, removes by-product impurity and waits refining.
There is no particular limitation for the melt viscosity of the pas resin that uses in this hair, considers at 310 ℃, velocity of shear 1000sec from formability
--1Under melt viscosity be 20～1200Pas, more preferably 200～1000Pas.Be especially in use under the injection molding situation, preferred molten viscosity is 20～200Pas, is used under the situation of extrusion moulding, and preferred molten viscosity is 200～1000Pas.
Then, use among the present invention do not contain crystal water, by chemical formula MgCO
3Shown magnesite is different with the material that is known as magnesiumcarbonate commonly used.The material that is known as magnesiumcarbonate commonly used is (3～5) MgCO
3Mg (OH)
2(3～7) H
2The basic salt that contains crystal water of O, hydroxyl magnesiumcarbonate.This hydroxyl magnesiumcarbonate is being heated to about 100 ℃, emits its crystal water, and in about 330 ℃ acutely decomposition of melting temperature of pas resin, problems such as foaming, decomposition appear in pas resin, can not be mixing.Do not contain crystal water, chemical formula is MgCO
3Magnesite, natural product, synthetics are arranged, because the impurity that contains in the natural product resolution problem may occur when mixing, so more preferably synthetics.
Synthetics obtains by handle above-mentioned hydroxyl magnesiumcarbonate under high temperature, high pressure, can not take place because the problem that crystal water or impurity cause.
The magnesite that makes by this method generally can obtain with high purity magnesite MSL, MSHP (refreshing island chemical industry (strain)).
And among the present invention, the addition of magnesite is very important, and addition can not show desired thermal conductivity very little, if opposite addition is too much, and the formability variation.Therefore, the addition of magnesite is 50～500 weight parts with respect to 100 weight part pas resins, is preferably 100～400 weight parts.
And the size distribution of magnesite is also very important, and median size is too little, and produce tackify when mixing with resin strong, the problem that has formability significantly to descend.Opposite particle diameter is too big, though thermal conductivity rises, can produce that mechanical properties descends or the problems such as superficiality variation during mold gate, extrusion moulding bad because of obstruction moulding during injection molding.Therefore, median size is 3～50 μ m, is preferably 5～25 μ m.
Then, as the alkoxysilane compound containing trialkylsilyl group in molecular structure that uses in the present invention, can be selected from aminoalkoxy silane, vinyl alkoxy silane, epoxy group(ing) organoalkoxysilane, sulfydryl organoalkoxysilane and allyl group organoalkoxysilane at least a.
As aminoalkoxy silane, so long as have more than one amino in a part, have the silane compound of 2 or 3 alkoxyl groups, any one is all effective, for example can enumerate gamma-amino propyl trimethoxy silicane, γ-An Jibingjisanyiyangjiguiwan, gamma-amino propyl group methyl dimethoxysilane, gamma-amino propyl group methyldiethoxysilane, N-(beta-aminoethyl)-gamma-amino propyl trimethoxy silicane, N-phenyl-gamma-amino propyl trimethoxy silicane etc.
As vinyl alkoxy silane, so long as have more than one vinyl in a part, have the silane compound of 2 or 3 alkoxyl groups, any one is all effective, for example can enumerate vinyltrimethoxy silane, vinyltriethoxysilane, vinyl three ('beta '-methoxy oxyethyl group) silane etc.
As the epoxy group(ing) organoalkoxysilane, so long as have more than one epoxy group(ing) in a part, have the silane compound of 2 or 3 alkoxyl groups, any one is all effective, γ-glycidyl propyl trimethoxy silicane, β-(3,4-epoxy group(ing) cyclohexyl) ethyl trimethoxy silane, γ-glycidyl propyl-triethoxysilicane etc. for example can have been enumerated.
As the sulfydryl organoalkoxysilane, so long as have more than one sulfydryl in a part, have the silane compound of 2 or 3 alkoxyl groups, any one is all effective, for example can enumerate γ-Qiu Jibingjisanjiayangjiguiwan, γ-sulfydryl propyl-triethoxysilicane etc.
As the allyl group organoalkoxysilane, so long as have more than one allyl group in a part, have the silane compound of 2 or 3 alkoxyl groups, any one is all effective, for example can enumerate can exemplify γ-diallyl TSL 8330, γ-allyl amino propyl trimethoxy silicane, γ-allyl sulfide are arranged for propyl trimethoxy silicane etc.
Among the present invention, aminoalkoxy silane most preferably in above-mentioned alkoxysilane compound containing trialkylsilyl group in molecular structure.
Among the present invention, the addition of alkoxysilane compound containing trialkylsilyl group in molecular structure is very important, and alkoxysilane compound containing trialkylsilyl group in molecular structure is few, and the mechanical properties behind the PCT significantly reduces, and the phase trans contents is too many, the resin tackify, and formability significantly reduces.Therefore, the addition of alkoxysilane compound containing trialkylsilyl group in molecular structure is 0.1～5 weight part with respect to 100 weight part pas resins, is preferably 0.5～4 weight part.
And, heat conductive resin composition of the present invention, within the scope of the present invention, in order to improve performances such as physical strength, thermotolerance, dimensional stability (anti-sex change, warpage), electrical property, also can cooperate inorganic or organic filler, here the different purpose of root a tree name is used fibrous, powder shape, flaky weighting agent.
As fibrous weighting agent, inorganic fibre shape materials such as glass fibre, fibrous magnesium silicate, boron fibre, potassium titanate fiber can have been enumerated.Fiber filling agent as representative is a glass fibre especially.In addition, also can use the organic fibrous matter of high-melting-points such as polymeric amide, fluoro-resin, acrylic resin.
On the other hand, as powder La shape weighting agent, can enumerate quartz powder, granulated glass sphere, glass powder, Calucium Silicate powder, pure aluminium silicate, kaolin, talcum powder, clay, diatomite, wollastonite class silicate, ferric oxide, titanium oxide, Zinc-oxide-based metal oxide, lime carbonate metalloid carbonate, calcium sulfate, barium sulfate metalloid vitriol.
And, as the sheet weighting agent, can enumerate mica, sheet glass.
These inorganic fillers can be used in combination more than a kind or 2 kinds.
And, the general known material that adds in thermoplastic resin is that stablizers such as tinting materials such as fire retardant, dyestuff or pigment, oxidation inhibitor or uv-absorbing agent, lubricant, crystallization promotor, crystallization nucleating agent etc. add aptly according to performance requriements, can be used as the present composition and uses.
Use the heat conductive resin composition of the present invention obtain like this, the moulding product that obtain by injection molding or extrusion moulding, blow molding etc. show high thermotolerance, chemical proofing, dimensional stability, flame retardant resistance, good exothermicity.Utilize this advantage, be suitable for inner produce heat release in the parts of outside such as heat exchanger, heat liberation board, light picker.
And, as other purposes, for example can enumerate family, the office electrical article parts of electrical and electronic parts such as being used for LED, transmitter, junctor, socket, terminal strip, printed base plate, motor part, ECU shell, illuminace component, TV part, cooker parts, microwave oven component, iron components, duplicating machine associated components, printer associated components, facsimile recorder associated components, well heater, idle call parts etc.
Embodiment
Below, with embodiment, comparative example the present invention is made specific description, but the invention is not restricted to these examples.In addition, the physical property measurement method among the embodiment is as follows.
(1) thermal conductivity
Use the sample of the discoideus moulding product of overlapping diameter 30mm, thick 2mm, measure thermal conductivity with hot dish method.
(2) injection molding
Be suitable for injection molding melt viscosity (310 ℃ of down cut speed are 1000sec using
-1) less than the resin combination of the pas resin of 200Pas, be 320 ℃ at barrel temperature, injection pressure is under the condition of 100M Pa, forms the bar-shaped moulding product of wide 20mm, thick 1mm, measures the distance that flows, as the evaluation of injection molding.
(3) extrusion moulding
(310 ℃ of down cut speed are 1000sec to using the melt viscosity that is suitable for extrusion moulding
-1) less than the resin combination of the pas resin of 200Pas, using barrel temperature is 330 ℃, goods in the pipe manufacturing usefulness of extrusion shaping machine mould top external diameter 6.3mm, internal diameter 5.7mm, with the extrusion capacity is that 20cc/min, pulling speed are 10m/min, during extrusion moulding, confirm to have or not the striped band of contraction and pipe, estimate extrusion moulding.
(4) humidity resistance
Use the iso standard test film of 80 * 10 * 4mm, under 121 ℃, humidity 100%, 2 atmospheric pressure, carry out pressure cooking test 48 hours, for this test film, carry out the mensuration of flexural strength according to ISO178, obtain conservation rate with respect to initial value.
(5) wear-resistant test
Use the iso standard test film of 80 * 10 * 4mm, use the cylinder of the SUS304 of Φ 10 * L20mm as compounding ingredient, the face of 80 * 4mm of contact iso standard test film on the periphery of SUS304 cylinder, in heavy burden 10kgf, speed is 3.5cm/sec, under the condition of stroke 5cm, after the iso standard test film comes and goes and repeats 20,000 times, measure the weight of iso standard test film and SUS304 cylinder, to estimate as abrasion loss with the difference of testing preceding weight.
Embodiment 1～4, comparative example 1～3
(310 ℃ of down cut speed are 1000sec to use melt viscosity
-1) less than the polyphenylene sulfide of 200Pas, thermal conductivity filler and alkoxysilane compound containing trialkylsilyl group in molecular structure, according to the composition shown in the table 1, use two forcing machines (the TEX30 α type that (strain) JSW makes) mixing, after forming mixing particle, utilize injection moulding machine to form above-mentioned test film, carry out various evaluations.The results are shown in the table 1.
Embodiment 5～8, comparative example 4～5
(310 ℃ of down cut speed are 1000sec to use melt viscosity
-1) less than polyphenylene sulfide, thermal conductivity filler and the alkoxysilane compound containing trialkylsilyl group in molecular structure of 200Pas, according to the composition shown in the table 2, use two forcing machines (the TEX30 α type that (strain) JSW makes) mixing, after forming mixing particle, utilize injection moulding machine to form above-mentioned test film, carry out various evaluations.And, above-mentioned extrusion moulding is estimated.The results are shown in the table 2.
In addition, each composition of use is as follows.
Polyphenylene sulfide (PPS resin)
The PPS-1:(strain) ((310 ℃ of down cut speed are 1000sec to melt viscosity to Network レ Ha corporate system Off オ one ト mouth Application W202A
-1) 25Pas)
((310 ℃ of down cut speed are 1000sec to melt viscosity to PPS-2 (strain) Network レ Ha corporate system Off オ one ト mouth Application W220A
-1) 220Pas)
The PPS-3:(strain) ((310 ℃ of down cut speed are 1000sec to melt viscosity to Network レ Ha corporate system Off オ one ト mouth Application W540
-1) 600Pas)
The thermal conductivity filler
Filler 1: (the high purity magnesite MSL of refreshing island chemical industry (strain) system, chemical formula is MgCO to magnesite
3, median size is 8 μ m)
Filler 2: (the high purity magnesite MSHP of refreshing island chemical industry (strain) system, chemical formula is MgCO to magnesite
3, median size is 22 μ m)
Filler 3 (relatively product): (the high-purity magnesium GP-30 of refreshing island chemical industry (strain) system, chemical formula is 4MgCO to magnesiumcarbonate
3Mg (OH)
24H
2O, median size is 9 μ m)
Filler 4 (relatively product): aluminum oxide (the spherical alumina AL203-05 of electrochemical industry (strain) system)
Filler 5 (relatively product): the magnesium oxide of coated with silica (Network one Le Off イ ラ one CF2-100 of テ ホ chemical industry (strain) system, median size is 27 μ m, maximum particle diameter is 100 μ m)
Alkoxysilane compound containing trialkylsilyl group in molecular structure: γ-An Jibingjisanyiyangjiguiwan.
Table 2
* 1: extrude and produce foaming and resin decomposition when mixing, can not be mixing
Claims (5)
1. heat conductive resin composition, wherein, with respect to the polyarylene sulfide resin of 100 weight parts, cooperate 50～500 weight parts do not contain crystal water, chemical formula MgCO
3Shown magnesite forms.
2. heat conductive resin composition as claimed in claim 1 wherein, with respect to the polyarylene sulfide resin of 100 weight parts, also cooperates the alkoxysilane compound containing trialkylsilyl group in molecular structure of 0.1～5 weight part to form.
3. highly thermal-conductive resin composition as claimed in claim 1 or 2, wherein, (310 ℃ of down cut speed are 1000sec to the melt viscosity of polyarylene sulfide resin
-1) be 20～1200Pas.
4. highly thermal-conductive resin composition as claimed in claim 1 or 2, wherein, (310 ℃ of down cut speed are 1000sec to the melt viscosity of polyarylene sulfide resin
-1) be 200～1000Pas
5. as any one the described heat conductive resin composition in the claim 1～4, wherein, the median size of magnesite is 3～50 μ m.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005298409A JP2007106854A (en) | 2005-10-13 | 2005-10-13 | Thermally conductive resin composition |
| JP298409/2005 | 2005-10-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101283049A true CN101283049A (en) | 2008-10-08 |
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ID=37942909
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800378220A Pending CN101283049A (en) | 2005-10-13 | 2006-10-12 | Thermally conductive resin composition |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2007106854A (en) |
| CN (1) | CN101283049A (en) |
| WO (1) | WO2007043695A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115698181A (en) * | 2020-06-02 | 2023-02-03 | Dic株式会社 | Polyarylene sulfide resin composition, molded article, and method for producing same |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4810963B2 (en) * | 2005-10-17 | 2011-11-09 | 東ソー株式会社 | Polyarylene sulfide composition |
| JP4929670B2 (en) * | 2005-10-17 | 2012-05-09 | 東ソー株式会社 | Polyarylene sulfide composition |
| JP5435494B2 (en) * | 2010-07-12 | 2014-03-05 | 協和化学工業株式会社 | Thickener |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2925930B2 (en) * | 1994-07-04 | 1999-07-28 | ポリプラスチックス株式会社 | Polyarylene sulfide resin composition |
| JP5031175B2 (en) * | 2002-12-26 | 2012-09-19 | ポリプラスチックス株式会社 | Polyarylene sulfide resin composition |
| JP4455911B2 (en) * | 2004-03-26 | 2010-04-21 | 神島化学工業株式会社 | Anhydrous magnesium carbonate filler, method for producing the same, and resin composition |
| JP2006160979A (en) * | 2004-12-10 | 2006-06-22 | Konoshima Chemical Co Ltd | Filler, its preparation and resin composition |
| JP4884691B2 (en) * | 2005-04-13 | 2012-02-29 | 神島化学工業株式会社 | Synthetic rubber composition |
-
2005
- 2005-10-13 JP JP2005298409A patent/JP2007106854A/en active Pending
-
2006
- 2006-10-12 CN CNA2006800378220A patent/CN101283049A/en active Pending
- 2006-10-12 WO PCT/JP2006/320792 patent/WO2007043695A1/en active Application Filing
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115698181A (en) * | 2020-06-02 | 2023-02-03 | Dic株式会社 | Polyarylene sulfide resin composition, molded article, and method for producing same |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2007043695A1 (en) | 2007-04-19 |
| JP2007106854A (en) | 2007-04-26 |
| WO2007043695A9 (en) | 2007-06-07 |
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Open date: 20081008 |