CN101448899B - Resin composition with high thermal conductivity - Google Patents
Resin composition with high thermal conductivity Download PDFInfo
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- CN101448899B CN101448899B CN200680054686.6A CN200680054686A CN101448899B CN 101448899 B CN101448899 B CN 101448899B CN 200680054686 A CN200680054686 A CN 200680054686A CN 101448899 B CN101448899 B CN 101448899B
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- thermal conductivity
- phosphorous
- high thermal
- resin composition
- magnesium oxide
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention claims a polyarylene resin material having no abrasion for crews and the like, high thermal conductivity, moldability and resistance to heat and humidity. Specifically peaking the invention relates to a resin composition with high thermal conductivity, 100-500 parts of phosphoric coating magnesia and 0.1-5 parts of alkoxy silane compound are mixed relative to 100 parts of polyarylene resin material.
Description
Technical field
The present invention relates to the resin composition with high thermal conductivity of formability excellence, humidity resistance excellence.
Background technology
With polyphenylene sulfide (below, sometimes abbreviate PPS as) resin be representative poly (arylene sulfide) (below, sometimes abbreviating PAS as) resin has high thermotolerance, mechanical properties, chemical proofing, dimensional stability, flame retardant resistance, therefore in electrical/electronic machine part material, automobile instrument component materials, chemical apparatus component materials etc., is extensive use of.In recent years, these compactization of parts, the heat radiation of the inside of parts etc. becomes problem, requires to have the material of thermal diffusivity.
Because this 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 this method can improve formability, but the Mohs' hardness of aluminum oxide is higher, therefore carrying out when mixing with resin or during moulding, having screw rod, cylinder or the forming mould heavy wear of forcing machine, shaper, the problem of tramp m..
On the other hand, proposed in the PPS resin, to cooperate graphite to give the method (JP-A 2003-41119) of heat conductivity, this method can not cause wear problems such as screw rod owing to filler, but when giving heat conductivity, also give electroconductibility, therefore had the problem that in requiring the field of electrical insulating property, to use.
Therefore, proposed with having an insulativity and thermal conductivity is higher and magnesium oxide that the Mohs' hardness ratio aluminum oxide is low adds as resin and uses the heat conductivity filler,, and in order to improve wet fastness that it is surperficial with silica-coated filler (JP-A 2003-34523).Yet, under the situation of using this filler, wet fastness under the normal temperature is improved, but the wet fastness under hot and humid (humidity resistance) deterioration, therefore, in the such test of pressure cooker testing (below, abbreviate PCT sometimes as), magnesium oxide is changed to magnesium hydroxide, exists to cause resin albefaction, expansion, the significantly reduced problem of mechanical properties.
Summary of the invention
The objective of the invention is to solve above-mentioned prior art problems, a kind of wear problem that does not have screw rod etc. is provided, and the high material of thermal conductivity of formability, humidity resistance excellence.
The inventor to achieve these goals, carry out meticulous research, found that pas resin is cooperated specific phosphorous lining magnesium oxide and alkoxysilane compound containing trialkylsilyl group in molecular structure simultaneously, then do not had the wear problem of screw rod etc., and formability, humidity resistance improve, thereby finish the present invention.
That is, the present invention is a kind of resin composition with high thermal conductivity, and it cooperates phosphorous lining magnesium oxide of 100～500 weight parts and 0.1～5 weight part alkoxysilane compound containing trialkylsilyl group in molecular structure to form by with respect to 100 weight part polyarylene sulfide resins.
Embodiment
Below, the present invention is described in detail.The pas resin that uses among the present invention mainly by as repeating unit-(Ar-S) (wherein, Ar is an arylidene) constitute.As arylidene, for example can use to phenylene, metaphenylene, adjacent phenylene, substituted phenylene, p p '-diphenylene sulfo group, p, p '-biphenylene, p, p '-diphenylene ether, p, p '-diphenylene carbonyl, naphthyl etc.In this case, in the arylene sulfide ether group that constitutes by above-mentioned arylidene, except the polymkeric substance that uses identical repeating unit, be the homopolymer, from the such viewpoint of the processibility of composition, the multipolymer that contains different repeat units also is preferred sometimes.
As homopolymer, preferred especially use with adopt to phenylene as arylidene to the poly (phenylene sulfide) ether group unitary material of attaching most importance to again.In addition,, in the arylene sulfide ether group that constitutes by above-mentioned arylidene, can use the different combinations of material more than 2 kinds, wherein, preferably especially use the combination that contains poly (phenylene sulfide) ether group and metaphenylene sulfide group as multipolymer.Wherein, the viewpoint on the rerum naturas such as thermotolerance, flowability (formability), mechanical characteristics is suitably for and contains more than the 70mol%, the above multipolymer to the poly (phenylene sulfide) ether group of preferred 80mol%.
In addition, in these pas resins, can especially preferably use the high-molecular weight polymer that is essentially straight chain structure that obtains as the monomer polycondensation of main body by with 2 functionality halogenated aromatic compounds, except the pas resin of straight chain structure, can use when polycondensation and to use monomer such as many halogen aromatics with 3 above halogenic substituents and part forms the polymkeric substance of branched structure or crosslinking structure on a small quantity, can also use straight chain structure polymkeric substance with lower molecular weight in the presence of oxygen or oxygenant, heating at high temperature and melt viscosity is risen and the polymkeric substance of improvement moulding processibility, or their mixture by oxidation cross-linked or heat cross-linking.
In addition, the pas resin that uses among the present invention can be with above-mentioned straight chain shape pas resin (310 ℃, velocity of shear 1200sec
-1Under viscosity be 10～300Pas) for main body, its a part (1～30 weight % is preferably 2～25 weight %) (300～3000Pas is preferably 500～2000Pas) the side chain or the mixed system of crosslinked pas resin for viscosity higher.In addition, the pas resin that uses among the present invention is preferably removed the impurity etc. of by-product and purifying by acid elution, hot wash, organic solvent washing (or their combination) etc. after polymerization.
Below, the so-called resin composition with high thermal conductivity of the present invention is the composition that cooperates phosphorous lining magnesium oxide and alkoxysilane compound containing trialkylsilyl group in molecular structure to form in above-mentioned pas resin.
The phosphorous lining magnesium oxide that uses among the present invention is that magnesium oxide and surface with the coating that is formed by the trimagnesium phosphate compounds have the coating that is formed by composite oxides, the magnesium oxide that its surperficial at least a portion also has the coating that is formed by the trimagnesium phosphate compounds.
Wherein, to have the magnesium oxide of the coating that is formed by composite oxides be that the element more than a kind in aluminium, iron, silicon and the titanium and the material of magnesium are contained in magnesian surface to what is called.As these composite oxides, specifically, forsterite (MgSi is arranged
4), spinel (Al
2Mg
4), magnesium ferrite (Fe
2MgO
4), magnesium titanate (MgTiO
3) etc., the preferably magnesium peridotites.
Below, the magnesian manufacture method of using among the present invention of phosphorous lining is described.
At first, the magnesian manufacture method in the magnesium oxide that uses in the magnesian manufacturing of phosphorous lining and the magnesium oxide with the coating that is formed by composite oxides is described.Magnesium oxide with characteristic of the present invention can use known method, for example manufacturing such as electro-dissolving, sintering process.
Below, magnesian manufacture method with the coating that is formed by composite oxides is: exist under the state of the compound that forms composite oxides on the magnesian surface of making by aforesaid method, fusion at high temperature, thus carry out the lining of composite oxides on the surface.As concrete method, can be after adding the compound that forms composite oxides by wet type in magnesium oxide powder, to mix stirring method; Or exist on magnesian surface under the state of the compound that forms composite oxides, the method for the sintering temperature more than the coating material fusing point is made.
The compound that is used to form composite oxides is preferably the compound more than a kind that is selected from the group that aluminum compound, iron cpd, silicon compound and titanium compound form.Form to compound is unqualified, can use nitrate, vitriol, muriate, oxynitrate, oxysulfate, oxygenated chlorinated thing, oxyhydroxide, oxide compound etc.As the object lesson of this compound, can enumerate aerosil, aluminum nitrate, iron nitrate etc.
The magnesian manufacture method of phosphorous lining is as follows: to the magnesium oxide by the aforesaid method manufacturing or have the magnesium oxide of the coating that is formed by composite oxides, carry out surface treatment by phosphorus compound, form coating on its surface by trimagnesium phosphate compounds.
As the phosphorus compound that in this surface treatment, uses, can enumerate phosphoric acid, phosphoric acid salt, phosphate ester acid etc., these materials can use separately, also can will use simultaneously more than 2 kinds.As phosphoric acid salt, can enumerate sodium phosphate, potassiumphosphate, ammonium phosphate etc., in addition, as phosphate ester acid, can enumerate acid p isopropylbenzoic acid base ester, acid methyl orthophosphoric acid, acid phosphate ester, acid phosphoric acid propyl ester, acid butyl phosphate, acid phosphoric acid Lauryl Ester, acid phosphoric acid stearyl, the own ester of acid phosphoric acid (2-ethyl), acid phosphoric acid oil base ester etc.Wherein, from the viewpoint of the coating of easy formation water tolerance excellence, preferred acid p isopropylbenzoic acid base ester.
Carry out the surface-treated concrete grammar as phosphorous lining is magnesian by phosphorus compound, be at magnesium oxide or have the phosphorus compound that adds specified amount in the magnesium oxide of the coating that forms by composite oxides, for example after stirring 5～60 minutes, under the temperature more than 300 ℃, sintering 0.5～5 hour and carrying out.
Phosphorous lining magnesium oxide by this method manufacturing can be purchased Network-Le Off イ ラ-CF2-100A (タ テ ホ chemical industry (strain) system) usually.
In addition, in the present invention, the magnesian addition of phosphorous lining is important, if addition is very few, then can't realize the thermal conductivity expected, and on the contrary, if addition is too much, then formability worsens.Therefore, the magnesian addition of phosphorous lining is 100～500 weight parts with respect to 100 weight part pas resins, is preferably 150～400 weight parts.
In addition, the magnesian size distribution of phosphorous lining also is important, if median size is too small, then with the mixing situation of resin under, can produce remarkable tackify, the significantly reduced problem of formability.On the contrary, if excessive, though then could exist thermal conductivity to improve the problem that mechanical properties reduces.In addition,, then when injection molding, can partly stop up filler particles, cause short problem such as penetrate at mould gate if maximum particle diameter is excessive.Therefore, as median size, be 10～50 μ m, be preferably 15～30 μ m, in addition, maximum particle diameter is preferably below the 150 μ m below 300 μ m.
Then, the alkoxysilane compound containing trialkylsilyl group in molecular structure that uses among the present invention is so long as be selected from least a getting final product in the group that aminoalkoxy silane, vinyl alkoxy silane, oxirane TMOS, sulfydryl organoalkoxysilane and allyl group organoalkoxysilane formed.
As aminoalkoxy silane, so long as have amino more than 1, as to have 2 or 3 alkoxyl groups silane compound in 1 molecule, just all be effectively, can enumerate for example 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 1 above vinyl in 1 molecule, have the silane compound of 2 or 3 alkoxyl groups, just all be effectively, can enumerate for example vinyltrimethoxy silane, vinyltriethoxysilane, vinyl three ('beta '-methoxy oxyethyl group) silane etc.
As the oxirane TMOS, so long as have 1 above epoxy group(ing) in 1 molecule, have the silane compound of 2 or 3 alkoxyl groups, be effective all just, can enumerate for example γ-glycidoxypropyltrime,hoxysilane, β-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxy propyl-triethoxysilicane etc.
As the sulfydryl organoalkoxysilane, so long as have 1 above sulfydryl in 1 molecule, have the silane compound of 2 or 3 alkoxyl groups, just all be effectively, can enumerate for example γ-Qiu Jibingjisanjiayangjiguiwan, γ-sulfydryl propyl-triethoxysilicane etc.
As the allyl group organoalkoxysilane, so long as have 1 above allyl group in 1 molecule, have the silane compound of 2 or 3 alkoxyl groups, just all be effectively, for example can enumerate γ-diallyl TSL 8330, γ-allyl amino propyl trimethoxy silicane, γ-allyl sulfide for propyl trimethoxy silicane etc.
In order to realize purpose of the present invention, in above-mentioned alkoxysilane compound containing trialkylsilyl group in molecular structure, aminoalkoxy silane most preferably.
In the present invention, the addition of alkoxysilane compound containing trialkylsilyl group in molecular structure is important, if alkoxysilane compound containing trialkylsilyl group in molecular structure is less, then the mechanical properties behind the PCT significantly reduces, on the contrary, if too much, resin tackify then, 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.
In addition, the manufacture method of resin composition with high thermal conductivity of the present invention can use (1) that whole raw materials are mixed and mixing method, (2) in pas resin, add alkoxysilane compound containing trialkylsilyl group in molecular structure, behind the melting mixing, add phosphorous lining method of magnesium oxide, (3) after making the pas resin fusion, add filler, the method of the filler that promptly in phosphorous lining magnesium oxide, adds alkoxysilane compound containing trialkylsilyl group in molecular structure and form etc., all methods all can embody effect of the present invention, owing to can improve physical strength by pas resin and alkoxysilane compound containing trialkylsilyl group in molecular structure reaction, therefore in order more effectively to make the reaction of pas resin and alkoxysilane compound containing trialkylsilyl group in molecular structure, preferably in pas resin, add alkoxysilane compound containing trialkylsilyl group in molecular structure by (2), behind the melting mixing, add the manufacturing of phosphorous lining method of magnesium oxide.
In addition, in purpose scope of the present invention, inorganic or the organic filler that can also cooperate character such as being used for improved mechanical strength, thermotolerance, dimensional stability (anti-distortion, warpage), electrical property in the resin composition with high thermal conductivity of the present invention, according to purpose, can also use fibrous, Powdered, tabular weighting agent therein.
As fibrous filler, can enumerate inorganic fibrous materials such as glass fibre, fibrous magnesium silicate, boron fibre, potassium titanate fiber.Representational especially fibrous filler is a glass fibre.In addition, can also use high-melting-point organic fibre materials such as polymeric amide, fluoro-resin, acrylic resin.
On the other hand, as Powdered weighting agent, can enumerate quartz powder, granulated glass sphere, glass powder, Calucium Silicate powder, pure aluminium silicate, kaolin, talcum, clay, diatomite, the so so so such metal sulfate of metal carbonate, calcium sulfate, barium sulfate of metal oxide, lime carbonate, magnesiumcarbonate of silicate, ferric oxide, titanium dioxide, zinc oxide of wollastonite.
In addition, as tabular weighting agent, can enumerate mica, sheet glass.
These inorganic fillers can use a kind or will be used in combination more than 2 kinds.
In addition, can also be according to performance requriements, suitably add the known material that in thermoplastic resin, adds usually, be stablizers such as tinting materials such as fire retardant, dyestuff or pigment, oxidation inhibitor or UV light absorber, lubricant, crystallization promotor, crystallization nucleating agent etc., such composition also can use as composition of the present invention.
Use thus obtained resin composition with high thermal conductivity of the present invention, demonstrate the thermal diffusivity of high humidity resistance, chemical proofing, dimensional stability, flame retardant resistance, excellence by the moulding product of acquisitions such as injection molding, extrusion moulding or blow molding.Utilize this advantage, can preferably in the parts that the outside sheds, use in heat exchanger, heating panel, the first-class heat that like this inside is produced of optics.
In addition, as other purposes, can also in for example families such as electrical/electronic components such as LED, transmitter, junctor, socket, terminal box, printed base plate, motor part, ECU box, illuminace component, TV part, the device component of cooking, microwave oven component, iron components, duplicating machine associated components, printer associated components, facsimile recorder associated components, well heater, idle call parts/company's electricity product component, use.
Embodiment
Below, by embodiment, comparative example the present invention is specifically described, but the present invention is not limited to this.In addition, the method for physical property measurement is as described below among the embodiment.
(1) thermal conductivity
Use is measured thermal conductivity by the overlapping sample that forms of discoideus moulding product of diameter 30mm, thickness 2mm by heat dish (Hot Disk) method.
(2) flowability
Under the condition of 340 ℃ of temperature cylinders, injection pressure 100MPa,, measure the distance that flows with the bar-shaped moulding product moulding of width 20mm, thickness 1mm.
(3) pliability test
Use the iso standard test film of 80 * 10 * 4mm, measure flexural strength and modulus in flexure according to ISO178.
(4) humidity resistance
Use the iso standard test film of 80 * 10 * 4mm, under 121 ℃, humidity 100%, 2 atmospheric conditions, carried out pressure cooker testing 48 hours,, this test film is carried out flexural strength measure, obtain conservation rate with respect to initial value according to ISO178.In addition, to the test film behind the pressure cooker testing, confirm according to X-ray diffraction analysis whether magnesium oxide is varied to magnesium hydroxide.
Embodiment 1～6, comparative example 1～5
According to composition shown in the table 1 and alkoxysilane compound containing trialkylsilyl group in molecular structure addition means, use twin screw extruder (the TEX30 α type that (strain) JSW makes), poly-p-phenylene sulfide ether resin, filler and alkoxysilane compound containing trialkylsilyl group in molecular structure carry out mixing, after forming particle, with above-mentioned test film moulding, carry out various evaluations by injection moulding machine.The result is shown in the table 1.
In addition, each composition of use and alkoxysilane compound containing trialkylsilyl group in molecular structure addition means are as described below.
Polyphenylene sulfide (PPS resin): Off オ-ト ロ Application W202A that Wu Yu chemical industry (strain) is made
Filler 1: phosphorous lining magnesium oxide, median size 27 μ m, maximum particle diameter 100 μ m (Network-Le Off イ ラ of タ テ ホ chemical industry (strain) manufacturing-CF2-100A)
Filler 2 (relatively product): silica-coated magnesium oxide, median size 27 μ m, maximum particle diameter 100 μ m (Network-Le Off イ ラ of タ テ ホ chemical industry (strain) manufacturing-CF2-100)
Organoalkoxysilane: γ-An Jibingjisanyiyangjiguiwan
(addition means of alkoxysilane compound containing trialkylsilyl group in molecular structure)
Method A: behind PPS resin and organoalkoxysilane melting mixing, add filler by the side feeder
Method B: behind melting mixing PPS resin, add the filler that has added organoalkoxysilane by the side feeder
Claims (5)
1. resin composition with high thermal conductivity, wherein, with respect to 100 weight part polyarylene sulfide resins, cooperate 100～500 weight parts to have median size 10～50 μ m, the phosphorous lining magnesium oxide and 0.1～5 weight part of the size distribution that maximum particle diameter 300 μ m are following are selected from aminoalkoxy silane, vinyl alkoxy silane, the oxirane TMOS, at least a alkoxysilane compound containing trialkylsilyl group in molecular structure in the group that sulfydryl organoalkoxysilane and allyl group organoalkoxysilane are formed, this phosphorous lining magnesium oxide are to be selected from phosphoric acid at the surface treatment procedure that is used for forming phosphorous coating on its surface in interpolation, carry out under the temperature more than 300 ℃ behind at least a phosphorus compound in phosphoric acid salt and the acid phosphoric acid ester that sintering forms.
2. resin composition with high thermal conductivity according to claim 1, wherein, phosphorous lining magnesium oxide has the coating that is formed by the trimagnesium phosphate compounds.
3. resin composition with high thermal conductivity according to claim 1, wherein, phosphorous lining mgo surface has the coating that is formed by composite oxides, also has the coating that is formed by the trimagnesium phosphate compounds on its surperficial at least a portion.
4. resin composition with high thermal conductivity according to claim 3, wherein, composite oxides contain more than one elements and the magnesium in aluminium, iron, silicon and the titanium.
5. the manufacture method of each described resin composition with high thermal conductivity of claim 1～4 is characterized in that, adds alkoxysilane compound containing trialkylsilyl group in molecular structure in polyarylene sulfide resin, and melting mixing adds phosphorous lining magnesium oxide then.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2006/310821 WO2007135749A1 (en) | 2006-05-24 | 2006-05-24 | Resin composition of high heat conduction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101448899A CN101448899A (en) | 2009-06-03 |
| CN101448899B true CN101448899B (en) | 2011-05-18 |
Family
ID=38723065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200680054686.6A Expired - Fee Related CN101448899B (en) | 2006-05-24 | 2006-05-24 | Resin composition with high thermal conductivity |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101448899B (en) |
| WO (1) | WO2007135749A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011010291A1 (en) * | 2009-07-24 | 2011-01-27 | Ticona Llc | Thermally conductive polymer compositions and articles made therefrom |
| KR101873139B1 (en) * | 2014-03-14 | 2018-06-29 | 다이니치 세이카 고교 가부시키가이샤 | Thermally conductive complex oxide, production method therefor, thermally conductive complex oxide-containing composition, and use therefor |
| CN104119587B (en) * | 2014-07-02 | 2016-03-30 | 合肥和安机械制造有限公司 | A kind of high temperature high voltage resistant hose material modified aluminium alumina and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001151905A (en) * | 1999-11-24 | 2001-06-05 | Tonen Chem Corp | Resin-made cooling body |
| CN1337980A (en) * | 1999-11-22 | 2002-02-27 | 协和化学工业株式会社 | Resin composition, molded article therefrom, and utilization thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01236270A (en) * | 1988-03-17 | 1989-09-21 | Showa Denko Kk | Resin composition |
| JP2878921B2 (en) * | 1993-03-03 | 1999-04-05 | ポリプラスチックス株式会社 | Polyarylene sulfide resin composition |
| JP3850371B2 (en) * | 2001-12-25 | 2006-11-29 | タテホ化学工業株式会社 | Resin composition containing magnesium oxide powder |
| JP2005264124A (en) * | 2004-03-22 | 2005-09-29 | Asahi Kasei Chemicals Corp | Polyphenylene sulfide resin composition |
-
2006
- 2006-05-24 CN CN200680054686.6A patent/CN101448899B/en not_active Expired - Fee Related
- 2006-05-24 WO PCT/JP2006/310821 patent/WO2007135749A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337980A (en) * | 1999-11-22 | 2002-02-27 | 协和化学工业株式会社 | Resin composition, molded article therefrom, and utilization thereof |
| JP2001151905A (en) * | 1999-11-24 | 2001-06-05 | Tonen Chem Corp | Resin-made cooling body |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101448899A (en) | 2009-06-03 |
| WO2007135749A1 (en) | 2007-11-29 |
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