CN103319893A - Preparation method of high-heat-conducting polyphenylene sulfide material and prepared material - Google Patents
Preparation method of high-heat-conducting polyphenylene sulfide material and prepared material Download PDFInfo
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- CN103319893A CN103319893A CN2013102898931A CN201310289893A CN103319893A CN 103319893 A CN103319893 A CN 103319893A CN 2013102898931 A CN2013102898931 A CN 2013102898931A CN 201310289893 A CN201310289893 A CN 201310289893A CN 103319893 A CN103319893 A CN 103319893A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method of a high-heat-conducting polyphenylene sulfide material and the prepared material. The preparation method aims at solving the problems that when conventional polyphenylene sulfide is processed, as cross linkage is easily caused, the regularity and the crystallinity of polyphenylene sulfide molecules are greatly reduced, the molecular large conjugated structure is damaged, the formation of a heat conduction channel is influenced, and the heat conduction property of polyphenylene sulfide resin is reduced. The preparation method comprises the steps of high-crystallinity polyphenylene sulfide resin preparation, high-heat-conducting fiber preparation and high-heat-conducting polyphenylene sulfide material preparation. The high-heat-conducting polyphenylene sulfide material prepared by the method has the characteristics that the using amount of heat-conducting packing is little, the heat-conducting coefficient is greater than 5w/m.k, and the overall performances such as mechanical property are excellent. As the high-heat-conducting polyphenylene sulfide material has the characteristics of high heat-conduction property and high heat resistance as well as excellent mechanical property, the high-heat-conducting polyphenylene sulfide material can be applied to structures and heat dissipation parts of electron devices such as LEDs (Light Emitting Diodes), LCD (Liquid Crystal Displays) and mobile phones.
Description
Technical field
The present invention relates to Material Field, polymeric material field especially is specially the material of a kind of highly heat conductive polyphenylene sulfide material preparation method and preparation.
Background technology
In recent years, along with developing rapidly of Electronic Assemblies technology and encapsulation technology, packing density significantly improves, and when thousands of times of electronic component and circuit volume dwindled, the relevant work frequency but sharply increased, thereby causes its job stability sharply to descend.For example in computer realm, along with the significantly raising of CPU running frequency and speed, the heat that CPU produces is multiplied.According to the Arhennius formula, 10 ℃ of the every risings of temperature, the life-span of electronic devices and components will reduce by 1/2.Therefore, still normally move under use temperature in order to guarantee CPU, and prolong its work-ing life, just the heat that produces must be left rapidly.
In field of aerospace, aircraft can be because friction produces a large amount of heats in flight course, and therefore, the safe flight of aircraft requires high to resistance toheat and the over-all properties of material.At present, the materials processing with good heat resistance energy is comparatively difficult, and expensive.If material has excellent heat dispersion, then just can be so not harsh to the requirement of its resistance toheat, processing also can become relatively easy.
At automotive field, in order to reduce car body weight, reduce car body noise and car body internal dust, make automobile more attractive in appearance, the spare and accessory parts such as the cylinder head cover of automobile, engine shield and air intake duct system generally adopt the plastics manufacturing.Because these type of spare and accessory parts such as cylinder head cover are nearer apart from engine, thereby temperature is higher.If the heat that engine can be produced leaves fast, will significantly improve the work-ing life of this type of part.
Therefore, the development heat conductivility is good, the polymer composite of excellent combination property, and design of material and expansion for fields such as electronics, aerospace and automobile makings have very important significance.The structure of polyphenylene sulfide is unique, and it has good high temperature resistant and thermostability, good chemical resistance, excellent physical and mechanical property, good gluing performance, good dimensional stability, good flame retardant resistance, good electrical property.Because polyphenylene sulfide has aforementioned many excellent properties, thereby so that it is widely used in machinery, electronics, chemical industry and aerospace field.Yet the thermal conductivity of polyphenylene sulfide is not high, has limited its application at field of radiating etc.Therefore, the development highly heat conductive polyphenylene sulfide composite material can be widened it in the application in the fields such as aerospace, chemical industry heat radiation.At present, disclosed heat conductive polyphenylene sulfide composite material mainly adopts the mode of heat conductive filler blend to be prepared.
Chinese patent application CN200810025883.6 is with polyphenylene sulfide, magnesium oxide, roving glass fiber, coupling agent, dispersion agent and lubricant blending extrusion by a certain percentage, and the thermal conductivity of prepared material is only up to 1.696W/m.K; Chinese patent application CN200810025884.0 utilizes zinc sulphide to prepare the anti-electrostatic heat conductive polyphenylene sulfide composite material for heat conductive filler, but the thermal conductivity of this material is no more than 1W/m.K; Chinese patent application CN1244887 utilizes graphite to prepare heat conductive polyphenylene sulfide composite material, and the elongation at break of this material is more than 10%, its range of application relative narrower; Chinese patent application 200710012359.8 utilizes carbon fiber, glass fibre, metal-powder, carbon black powder and mineral filler to prepare heat-conducting polyphenyl thioether material, heat-conductivity conducting Material Addition amount is 10 ~ 25% in the prepared material, but its toughness is still undesirable; Chinese patent application CN201110261250.7 utilizes nano level heat-conducting metal filamentary material, inorganic filling material, conductive powder powder material and ceramic alumina fiber to prepare a kind of heat conductive polyphenylene sulfide composite material, then in this material, steel fiber density is larger, so that this quality of materials is heavier; Chinese patent application 201210051775.2 adopts thermal conducting agent NP325, coupling agent, toughner, graft modification agent, stablizer and other auxiliary agent to prepare the polyphenyl thioether composite material that a kind of thermal conductivity is 11.2W/m.K, this material has preferably toughness, but its intensity is difficult to use as structured material.
Simultaneously, other thermal conductivity thermoplastic materials also mainly adopt the mode of heat conductive filler blend to be prepared, and are as follows.Chinese patent ZL99815810.0 cooperates highdensity metal, metal oxide as filler with carbon fiber and the boron nitride of high length-diameter ratio, and the thermal conductivity of prepared product is 20W/m.K; As filler, the thermal conductivity of prepared product is between 2 ~ 4W/m.K with insulating packings such as metal oxide, silicon nitrides for Chinese patent ZL200510101700.0; Chinese patent ZL02112481.7 prepares heat-conductive composite material with various ceramic fibers or Graphite Powder 99 or carbon black or carbon fiber or metal powder combination as filler; Chinese patent application numbers 201010228254.0 utilizes nano aluminium oxide to be heat conductive filler, has prepared high-heat-conductive composite material take polyethylene and EVA as matrix, and the thermal conductivity of this material is lower than 1W/m.K, and is still lower; Chinese patent application 201110008919.1 with mass ratio be the fibrous heat conductive filler of 1:1 ~ 1:200 and Graphene as thermal conducting agent, prepared thermally conductive material, the thermal conductivity maximum of this thermally conductive material is 3.36W/m.K, its tensile strength only is 34MPa; Chinese patent application 201010234818.1 utilizes β-SiCw/ β-SiCp as heat conductive filler, adopts the mixing heat conduction poly styrene composite material that prepared of open type dual-roller, and the thermal conductivity of this material is up to 1.29W/m.K; The graphene nanometer sheet that Chinese patent application 201210269880.3 obtains behind the natural graphite ball milling adopts the method for stamping of powder to prepare the heat conduction nylon 66 composite material as heat conductive filler, and the thermal conductivity of this material is up to 3.86W/m.K; Chinese patent application 201210237383.5 has prepared the heat conduction polytetrafluoroethylmaterial material with graphite and carbon fiber as heat conductive filler, but the thermal conductivity of this material is no more than 1W/m.K; Chinese patent application 201210190402.3 has prepared the heat conduction polypropylene composite material take expanded graphite as heat conductive filler, when the thermal conductivity of this material reached the highest 1.82W/m.K, its tensile strength only was 23.5MPa; Chinese patent CN201110245020.1 utilizes aluminium nitride powder to prepare insulating heat-conductive ABS matrix material, but the thermal conductivity of this material is no more than 1W/m.K.
Make a general survey of above-mentioned patent, the heat conductive filler of selecting mostly is greatly graphite, carbon fiber, aluminum oxide, boron nitride, silicon carbide, metal-powder and fiber etc.For the powdery type heat conductive filler of metal oxide, nitride and graphite-like, it is when forming the heat conduction network, and the large usage quantity of heat conductive filler causes it the problems such as mechanical properties decrease, processing difficulties to occur usually.And for the heat conductive filler of metal-powder and fiber-like, because the density of this metalloid and the density of macromolecular material differ larger, so that its easily layering in the batch mixing process is difficult to realize blend processing.For the heat conductive fillers such as carbon fiber, it easily forms the heat conduction network, but himself thermal conductivity is relatively low.Simultaneously, existing disclosed patent mostly concentrates on selects different heat conductive fillers to prepare heat-conductive composite material, and for how improving in the heat-conductive composite material, the thermal conductivity of body material rarely has report.
Utilizing the synthetic macromolecular material with conjugated structure of electronics transmission or phonon thermal conduction mechanism, is one of effective way of the high heat-conducting polymer material of preparation.The molecular structure of polyphenylene sulfide is fairly simple, and its molecular backbone chain is formed by phenyl ring and sulphur atom alternative arrangement, and the lone electron on the sulphur atom can form large conjugated structure with phenyl ring, can improve the thermal conductivity of polyphenylene sulfide.But polyphenylene sulfide is adding man-hour, easily occurs crosslinkedly, greatly reduces regularity and the degree of crystallinity of polyphenylene sulfide molecule, has destroyed the large conjugated structure of molecule, has affected the formation of passage of heat, has reduced the thermal conductivity of polyphenylene sulfide.
Summary of the invention
Goal of the invention of the present invention is: adding man-hour for existing polyphenylene sulfide, easily occur crosslinked, greatly reduce regularity and the degree of crystallinity of polyphenylene sulfide molecule, destroyed the large conjugated structure of molecule, affected the formation of passage of heat, reduced the problem of the thermal conductivity of polyphenylene sulfide, the material of a kind of highly heat conductive polyphenylene sulfide material preparation method and preparation is provided.Adopt the highly heat conductive polyphenylene sulfide material of the inventive method preparation, have a heat conductive filler consumption low, thermal conductivity is greater than 5w/ (m.k), the characteristics of the excellent combination properties such as mechanics.Because this material has high heat conduction, high heat-resisting characteristic, and mechanical property is excellent, thereby can be used in structure and the thermal component of the electron devices such as LED, LCD and mobile phone.
To achieve these goals, the present invention adopts following technical scheme:
A kind of highly heat conductive polyphenylene sulfide material preparation method comprises the steps:
(1) preparation high-crystallinity polyphenylene sulfide
Take by weighing respectively each component by following ratio of weight and number: 90-99 part linear polyphenylene sulfide resin, 1-10 part stablizer, 0.5-1.5 part oxidation inhibitor, linear polyphenylene sulfide resin, stablizer, the oxidation inhibitor that takes by weighing is added in the stirrer of preparing burden at a high speed, mix, get a Preblend;
A Preblend is placed dual-screw-stem machine, a Preblend melt extrudes through dual-screw-stem machine, again through cooling, dry, granulation, get granular high-crystallinity polyphenylene sulfide, wherein, the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃;
(2) prepare high heat conducting fiber
Adopt a kind of in electroless plating method, chemical Vapor deposition process, pulsed laser deposition, sol-gel surface-coated method, the ion sputtering film coating method, plated surface last layer metallic membrane at carbon fiber, get high heat conducting fiber, the thickness of described metallic membrane is 0.05-0.30 μ m;
(3) preparation highly heat conductive polyphenylene sulfide material
Take by weighing respectively the component of following ratio of weight and number: high heat conducting fiber, 20-30 part crystalline thermoplastic resin of the high-crystallinity polyphenylene sulfide of 30-50 part step (1) preparation, 20-50 part step (2) preparation, the high-crystallinity polyphenylene sulfide that takes by weighing, high heat conducting fiber, crystalline thermoplastic resin are added in the stirrer of preparing burden at a high speed, mix, get secondary Preblend;
Secondary Preblend is placed single-screw machine, secondary Preblend melt extrudes through single-screw machine, again through cooling, granulation, get the highly heat conductive polyphenylene sulfide material, wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃.
In the described step (3), crystalline thermoplastic resin is a kind of of nylon 66, polyether-ether-ketone, polypropylene, polyester.
In the described step (1); oxidation inhibitor is β-(3; the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, four [β-(3; the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) one or more in hexanediamine, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
In the described step (1), stablizer is one or more in the bi-imidazoline nitrone oxynitride, line style nitrone class, annular nitrone class of polyether chain bridged.
In the described step (1), stablizer is α, one or more in ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers, cyclic chiral alpha-alkyl carbonyl nitre copper, the line style nitrone class.
In the described step (1), linear polyphenylene sulfide resin, stablizer, the oxidation inhibitor that takes by weighing is added in the stirrer of preparing burden at a high speed, mix, the rotating speed of the stirrer of preparing burden at a high speed is 480-960 r/min, and mixing time is 3-5 min, gets a Preblend.
In the described step (1), adopt water-cooled to cool off, adopt hot blast to carry out drying.
In the described step (1), adopt dicing machine to carry out granulation, the rotating speed of dicing machine is 300-500 r/min.
In the described step (2), adopt a kind of metallic membrane for preparing in copper, silver, aluminium, nickel, the zirconium.
In the described step (2), carbon fiber is chopped asphalt base carbon fiber.
In the described step (3), the high-crystallinity polyphenylene sulfide that takes by weighing, high heat conducting fiber, crystalline thermoplastic resin are added in the stirrer of preparing burden at a high speed, mix, get secondary Preblend, wherein, the rotating speed of the stirrer of preparing burden at a high speed is 480-960 r/min, and mixing time is 2-4 min.
In the described step (3), secondary Preblend is placed single-screw machine, secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, gets the highly heat conductive polyphenylene sulfide material.
Adopt the material of aforementioned highly heat conductive polyphenylene sulfide material preparation method preparation.
The invention provides the material of a kind of highly heat conductive polyphenylene sulfide material preparation method and preparation, compare with conventional preparation method, the present invention has increased the surface treatment of poly-p-phenylene sulfide ether resin (being the PPS resin) linearization process, heat conductive filler, has also adopted simultaneously Double substrate micro interface heat conduction technology.The Double substrate micro interface heat conduction technology that adopts in the step of the present invention (3), utilize two kinds of incompatible polymers can form interface structure, thereby allow the heat conduction network between two kinds of polymer interfaces, form, can effectively put forward heat conduction efficiency, thereby can reduce the consumption of heat conductive filler.
Among the present invention, at first by preparation high-crystallinity polyphenylene sulfide technology, solve the crosslinked problem of polyphenylene sulfide in the course of processing, guaranteed the regularity of its molecule, prevented the reduction of resin thermal conductivity; Simultaneously, the technology of preparing by high heat conducting fiber has solved the hot relatively poor problem of carbon fiber guiding; And utilize Double substrate micro interface heat conduction technology in the step (3), prepare low, the high heat conduction of heat conductive filler consumption, and the highly heat conductive polyphenylene sulfide material of excellent combination property.
Embodiment
Disclosed all features in this specification sheets, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Disclosed arbitrary feature in this specification sheets is unless special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, unless special narration, each feature is an example in a series of equivalences or the similar characteristics.
Embodiment 1
(1) preparation high-crystallinity polyphenylene sulfide
The linear polyphenylene sulfide resin is in 130 ℃ of lower baking 3 h, for subsequent use.Take by weighing respectively 95 kg linear polyphenylene sulfide resins, 4 kg α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and 1 kg β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, with linear polyphenylene sulfide resin, α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid adds in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 3-5 min, gets a Preblend.
A Preblend is placed dual-screw-stem machine; a Preblend melt extrudes through dual-screw-stem machine; again after cooling by water, warm air drying, dicing machine shear granulation; get the pelletizing of high-crystallinity polyphenylene sulfide; wherein; the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
(2) prepare high heat conducting fiber
Get the chopped asphalt base carbon fiber of 50kg, the employing electroless plating method is 0.05 ~ 0.30 micron metallic copper in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.Concrete operation step is as follows.
Get the chopped asphalt base carbon fiber of 50kg, place air, at 400 ℃ of lower calcination 20min, remove glue and other organism on chopped asphalt base carbon fiber surface by the mode of calcination oxidation, get fiber calcination thing.It is 20% HNO that fiber calcination thing is placed massfraction
3Boil 10min in the solution and carry out alligatoring, then rinse well with the fiber calcination thing of deionized water after with alligatoring, placing massfraction is 20% SnCl again
2Boil 5min in the solution and carry out sensitization, rinse well with deionized water, then placing massfraction is 0.5% AgNO
3In the solution, stir 5min and activate, rinse well with deionized water again, get pretreated fiber.
Get 40kg zinc powder, 0.5kg dodecyl soap, for subsequent use.Zinc powder, dodecyl soap, pretreated fiber are added in the batching stirrer, the rotating speed of batching stirrer is 480-600 r/min, after stirring 2-4 min, add again the 100kg massfraction in the batching stirrer and be 5% copper-bath, reduce stirring velocity, stirring at low speed 5min gets the Cu coated fibre crude green body.Be that 2% benzotriazole solution carries out Passivation Treatment with Cu coated fibre crude green body massfraction, clean up with deionized water again, get Cu coated fibre passivation base.Cu coated fibre passivation base at 100 ℃ of lower oven dry 2h, is got high heat conducting fiber.
(3) preparation highly heat conductive polyphenylene sulfide material dries by the fire 3 h with the high-crystallinity polyphenylene sulfide of nylon 66 and step (1) preparation under 130 ℃, and is for subsequent use.Take by weighing respectively the high heat conducting fiber of high-crystallinity polyphenylene sulfide after the 45 kg oven dry, the nylon 66 after the 20 kg oven dry, 35kg step (2) preparation, these three kinds of components are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.
Secondary Preblend is placed single-screw machine, and secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, and the particle packing after the granulation gets the highly heat conductive polyphenylene sulfide material.Wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
Embodiment 2
(1) preparation high-crystallinity polyphenylene sulfide
The linear polyphenylene sulfide resin is in 130 ℃ of lower baking 3 h, for subsequent use.Take by weighing respectively 95 kg linear polyphenylene sulfide resins, 4 kg α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and 1 kg β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, with linear polyphenylene sulfide resin, α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid adds in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 3-5 min, gets a Preblend.
A Preblend is placed dual-screw-stem machine; a Preblend melt extrudes through dual-screw-stem machine; after again cooling, drying, the dicing machine shear granulation; get granular high-crystallinity polyphenylene sulfide; wherein; the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
(2) prepare high heat conducting fiber
Get the chopped asphalt base carbon fiber of 50kg, the employing electroless plating method is 0.05 ~ 0.30 micron metallic copper in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.Concrete operation step is as follows.
Get the chopped asphalt base carbon fiber of 50kg, place air, at 400 ℃ of lower calcination 20min, remove glue and other organism on chopped asphalt base carbon fiber surface by the mode of calcination oxidation, get fiber calcination thing.It is 20% HNO that fiber calcination thing is placed massfraction
3Boil 10min in the solution and carry out alligatoring, then rinse well with the fiber calcination thing of deionized water after with alligatoring, placing massfraction is 20% SnCl again
2Boil 5min in the solution and carry out sensitization, rinse well with deionized water, then placing massfraction is 0.5% AgNO
3In the solution, stir 5min and activate, rinse well with deionized water again, get pretreated fiber.
Get 40kg zinc powder, 0.5kg dodecyl soap, for subsequent use.Zinc powder, dodecyl soap, pretreated fiber are added in the batching stirrer, the rotating speed of batching stirrer is 480-600 r/min, after stirring 2-4 min, add again the 100kg massfraction in the batching stirrer and be 5% copper-bath, reduce stirring velocity, stirring at low speed 5min gets the Cu coated fibre crude green body.Be that 2% benzotriazole solution carries out Passivation Treatment with Cu coated fibre crude green body massfraction, clean up with deionized water again, get Cu coated fibre passivation base.Cu coated fibre passivation base at 100 ℃ of lower oven dry 2h, is got high heat conducting fiber.
(3) preparation highly heat conductive polyphenylene sulfide material
With high-crystallinity polyphenylene sulfide baking 3 h under 130 ℃ of nylon 66 and step (1) preparation, for subsequent use.Take by weighing respectively the high heat conducting fiber of high-crystallinity polyphenylene sulfide after the 35 kg oven dry, the nylon 66 after the 20 kg oven dry, 45kg step (2) preparation, high-crystallinity polyphenylene sulfide, nylon 66, these three kinds of components of high heat conducting fiber are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.
Secondary Preblend is placed single-screw machine, and secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, and the particle packing after the granulation gets the highly heat conductive polyphenylene sulfide material.Wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
Embodiment 3
(1) preparation high-crystallinity polyphenylene sulfide
The linear polyphenylene sulfide resin is in 130 ℃ of lower baking 3 h, for subsequent use.Take by weighing respectively 95 kg linear polyphenylene sulfide resins, 4 kg α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and 1 kg β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, with linear polyphenylene sulfide resin, α, ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers and β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid adds in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 3-5 min, gets a Preblend.
A Preblend is placed dual-screw-stem machine, and a Preblend melt extrudes through dual-screw-stem machine, after cooling by water, warm air drying, dicing machine shear granulation, gets granular high-crystallinity polyphenylene sulfide again.Wherein, the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
(2) prepare high heat conducting fiber
Get the chopped asphalt base carbon fiber of 50kg, employing ion sputtering film coating method is 0.05 ~ 0.30 micron metallic copper in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.What the ion sputtering film coating method adopted is FJ-5 type magnetron sputtering coater, and magneticstrength is 80 ~ 200Gs, and Ar pressure is 2 * 10
-1Pa, sputtering voltage are 200～600V, and vacuum tightness is 6.5 * 10
-5Pa.
(3) preparation highly heat conductive polyphenylene sulfide material
With high-crystallinity polyphenylene sulfide baking 3 h under 130 ℃ of nylon 66 and step (1) preparation, for subsequent use.Take by weighing respectively the high heat conducting fiber of high-crystallinity polyphenylene sulfide after the 35 kg oven dry, the nylon 66 after the 20 kg oven dry, 45kg step (2) preparation, high-crystallinity polyphenylene sulfide, nylon 66, these three kinds of components of high heat conducting fiber are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.
Secondary Preblend is placed single-screw machine, and secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, and the particle packing after the granulation gets the highly heat conductive polyphenylene sulfide material.Wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
Embodiment 4
(1) preparation high-crystallinity polyphenylene sulfide
The linear polyphenylene sulfide resin is in 130 ℃ of lower baking 3 h, for subsequent use.Take by weighing respectively 90 kg linear polyphenylene sulfide resins, 9 kg cyclic chiral alpha-alkyl carbonyl nitre copper and 1 kg four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, these three kinds of components are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 3-5 min, gets a Preblend.Wherein, cyclic chiral alpha-alkyl carbonyl nitre copper is bought from Sichuan Coremer Materials Ltd..
A Preblend is placed dual-screw-stem machine, and a Preblend melt extrudes through dual-screw-stem machine, after cooling by water, warm air drying, dicing machine shear granulation, gets granular high-crystallinity polyphenylene sulfide again.Wherein, the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
(2) prepare high heat conducting fiber
Get the chopped asphalt base carbon fiber of 50kg, employing ion sputtering film coating method is 0.05 ~ 0.30 micron metallic copper in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.What the ion sputtering film coating method adopted is FJ-5 type magnetron sputtering coater, and magneticstrength is 80 ~ 200Gs, and Ar pressure is 2 * 10
-1Pa, sputtering voltage are 200～600V, and vacuum tightness is 6.5 * 10
-5Pa.
(3) preparation highly heat conductive polyphenylene sulfide material
With high-crystallinity polyphenylene sulfide baking 3 h under 130 ℃ of polyether-ether-ketone and step (1) preparation, for subsequent use.Take by weighing respectively the high heat conducting fiber of high-crystallinity polyphenylene sulfide after the 40 kg oven dry, the polyether-ether-ketone after the 20 kg oven dry, 40kg step (2) preparation, high-crystallinity polyphenylene sulfide, polyether-ether-ketone, these three kinds of components of high heat conducting fiber are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.
Secondary Preblend is placed single-screw machine, and secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, and the particle packing after the granulation gets the highly heat conductive polyphenylene sulfide material.Wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
Embodiment 5
(1) preparation high-crystallinity polyphenylene sulfide
The linear polyphenylene sulfide resin is in 130 ℃ of lower baking 3 h, for subsequent use.Take by weighing respectively 94 kg linear polyphenylene sulfide resins, 2.5 kg α; ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers, 2.5 kg line style nitrone class stablizers, 0.5 kg N; N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine and 0.5 kg four [β-(3; the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester; these five kinds of components are added in the stirrer of preparing burden at a high speed; mix; the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min; mixing time is 3-5 min, gets a Preblend.Wherein, line style nitrone class stablizer is bought from Sichuan Coremer Materials Ltd..
A Preblend is placed dual-screw-stem machine, and a Preblend melt extrudes through dual-screw-stem machine, after cooling by water, warm air drying, dicing machine shear granulation, gets granular high-crystallinity polyphenylene sulfide again.Wherein, the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
(2) prepare high heat conducting fiber
Get the chopped asphalt base carbon fiber of 50kg, employing ion sputtering film coating method is 0.05 ~ 0.30 micron metallic nickel in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.What the ion sputtering film coating method adopted is FJ-5 type magnetron sputtering coater, and magneticstrength is 80 ~ 200Gs, and Ar pressure is 2 * 10
-1Pa, sputtering voltage are 200～600V, and vacuum tightness is 6.5 * 10
-5Pa.
(3) preparation highly heat conductive polyphenylene sulfide material
With high-crystallinity polyphenylene sulfide baking 3 h under 130 ℃ of polybutylene terephthalate and step (1) preparation, for subsequent use.Take by weighing respectively the high heat conducting fiber of high-crystallinity polyphenylene sulfide after the 30 kg oven dry, the polybutylene terephthalate after the 30 kg oven dry, 40kg step (2) preparation, high-crystallinity polyphenylene sulfide, polybutylene terephthalate, these three kinds of components of high heat conducting fiber are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.
Secondary Preblend is placed single-screw machine, and secondary Preblend melt extrudes through single-screw machine, and the material of extruding is sent into granulation in the dicing machine after immersing and cooling off in the tank, and the particle packing after the granulation gets the highly heat conductive polyphenylene sulfide material.Wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃; main frame frequency: 20-35Hz; feeding frequency: 10-15Hz, the rotating speed of dicing machine are 300-500 r/min.
Embodiment 6
In the high heat conducting fiber of step (2) preparation: get the chopped asphalt base carbon fiber of 50kg, employing ion sputtering film coating method is 0.05 ~ 0.30 micron metallic aluminium in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.Other are identical with embodiment 3.
Embodiment 7
In the high heat conducting fiber of step (2) preparation: get the chopped asphalt base carbon fiber of 50kg, employing ion sputtering film coating method is 0.05 ~ 0.30 micron argent in chopped asphalt base carbon fiber plated surface a layer thickness, gets high heat conducting fiber.Other are identical with embodiment 3.
Embodiment 8
In step (3) the preparation highly heat conductive polyphenylene sulfide material, do not add 20kg crystalline thermoplastic resin nylon 66, that is: with high-crystallinity polyphenylene sulfide baking 3 h under 130 ℃ of step (1) preparation, for subsequent use.Take by weighing respectively the high-crystallinity polyphenylene sulfide after 55 kg are dried, the high heat conducting fiber of 45kg step (2) preparation, high-crystallinity polyphenylene sulfide, these two kinds of components of high heat conducting fiber are added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, mixing time is 2-4 min, gets secondary Preblend.Other are identical with embodiment 3.
Embodiment 9
Adopt three (2,4-di-tert-butyl-phenyl) phosphorous acid ester of equal in quality to substitute β-(3,5-di-t-butyl-4-hydroxybenzene) propionic acid octadecanol ester, other are identical with embodiment 2.
Highly heat conductive polyphenylene sulfide material to embodiment 1-8 preparation is tested, and the performance test results is as follows.
The highly heat conductive polyphenylene sulfide material of embodiment 1 preparation: tensile strength is 125MPa, and flexural strength is 221MPa, and modulus in flexure is 23.4GPa, and the socle girder notched Izod impact strength is 6.8KJ.m
-2, thermal conductivity is 8.13W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 2 preparations: tensile strength is 113MPa, and flexural strength is 210MPa, and modulus in flexure is 19.3GPa, and the socle girder notched Izod impact strength is 6.0KJ.m
-2, thermal conductivity is 12.34W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 3 preparations: tensile strength is 118MPa, and flexural strength is 216MPa, and modulus in flexure is 21.0GPa, and the socle girder notched Izod impact strength is 7.3KJ.m
-2, thermal conductivity is 16.32W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 4 preparations: tensile strength is 124MPa, and flexural strength is 221MPa, and modulus in flexure is 23.6GPa, and the socle girder notched Izod impact strength is 6.9KJ.m
-2, thermal conductivity is 13.12W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 5 preparations: tensile strength is 119MPa, and flexural strength is 218MPa, and modulus in flexure is 20.6GPa, and the socle girder notched Izod impact strength is 6.5KJ.m
-2, thermal conductivity is 13.95W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 6 preparations: tensile strength is 120MPa, and flexural strength is 215MPa, and modulus in flexure is 19.3GPa, and the socle girder notched Izod impact strength is 6.9KJ.m
-2, thermal conductivity is 6.92W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 7 preparations: tensile strength is 120MPa, and flexural strength is 217MPa, and modulus in flexure is 20.7GPa, and the socle girder notched Izod impact strength is 7.5KJ.m
-2, thermal conductivity is 21.80W (mK)
-1
The highly heat conductive polyphenylene sulfide material of embodiment 8 preparations: tensile strength is 124MPa, and flexural strength is 220MPa, and modulus in flexure is 19.4GPa, and the socle girder notched Izod impact strength is 6.6KJ.m
-2, thermal conductivity is 12.00W (mK)
-1
Experimental result by above-described embodiment can be found out: embodiment 2 and embodiment 3 contrast and can find, the ion sputtering film coating method is better than electroless plating method, so that the thermal conductivity of matrix material is higher; Embodiment 3 and embodiment 6,7 contrast and can find, the thermal conductivity of coated metal just is directly connected to the thermal conductivity of composite materials height of last gained; Embodiment 3 and embodiment 8 contrasts can find that the Double substrate micro interface tech that step of the present invention (3) adopts has large help for the heat conductivility that improves material.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (10)
1. a highly heat conductive polyphenylene sulfide material preparation method is characterized in that, comprises the steps:
(1) preparation high-crystallinity polyphenylene sulfide
Take by weighing respectively each component by following ratio of weight and number: 90-99 part linear polyphenylene sulfide resin, 1-10 part stablizer, 0.5-1.5 part oxidation inhibitor, linear polyphenylene sulfide resin, stablizer, the oxidation inhibitor that takes by weighing is added in the stirrer of preparing burden at a high speed, mix, get a Preblend;
A Preblend is placed dual-screw-stem machine, a Preblend melt extrudes through dual-screw-stem machine, again through cooling, dry, granulation, get granular high-crystallinity polyphenylene sulfide, wherein, the temperature setting of dual-screw-stem machine is set to: one section temperature 240-260 ℃, two sections temperature 255-275 ℃, three sections temperature 260-275 ℃, four sections temperature 265-275 ℃, five sections temperature 280-300 ℃;
(2) prepare high heat conducting fiber
Adopt a kind of in electroless plating method, chemical Vapor deposition process, pulsed laser deposition, sol-gel surface-coated method, the ion sputtering film coating method, plated surface last layer metallic membrane at carbon fiber, get high heat conducting fiber, the thickness of described metallic membrane is 0.05-0.30 μ m;
(3) preparation highly heat conductive polyphenylene sulfide material
Take by weighing respectively the component of following ratio of weight and number: high heat conducting fiber, 20-30 part crystalline thermoplastic resin of the high-crystallinity polyphenylene sulfide of 30-50 part step (1) preparation, 20-50 part step (2) preparation, the high-crystallinity polyphenylene sulfide that takes by weighing, high heat conducting fiber, crystalline thermoplastic resin are added in the stirrer of preparing burden at a high speed, mix, get secondary Preblend;
Secondary Preblend is placed single-screw machine, secondary Preblend melt extrudes through single-screw machine, again through cooling, granulation, get the highly heat conductive polyphenylene sulfide material, wherein, the temperature setting of single-screw machine is set to: one section temperature 260-320 ℃, two sections temperature 265-325 ℃, three sections temperature 270-330 ℃, four sections temperature 275-335 ℃, five sections temperature 280-320 ℃.
2. described highly heat conductive polyphenylene sulfide material preparation method according to claim 1 is characterized in that, in the described step (3), crystalline thermoplastic resin is a kind of of nylon 66, polyether-ether-ketone, polypropylene, polyester.
3. described highly heat conductive polyphenylene sulfide material preparation method according to claim 1 and 2; it is characterized in that; in the described step (1); oxidation inhibitor is β-(3; the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, N, N'-pair-(3-(3; the 5-di-tert-butyl-hydroxy phenyl) propionyl) one or more in hexanediamine, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
4. described highly heat conductive polyphenylene sulfide material preparation method according to claim 3 is characterized in that, in the described step (1), stablizer is one or more in the bi-imidazoline nitrone oxynitride, line style nitrone class, annular nitrone class of polyether chain bridged.
5. described highly heat conductive polyphenylene sulfide material preparation method according to claim 3, it is characterized in that, in the described step (1), stablizer is α, one or more in ω-two (tetrahydroglyoxaline nitrone nitrogen oxygen) phenyl polyethers, cyclic chiral alpha-alkyl carbonyl nitre copper, the line style nitrone class.
6. according to claim 1,2,4,5 each described highly heat conductive polyphenylene sulfide material preparation methods, it is characterized in that, in the described step (1), linear polyphenylene sulfide resin, stablizer, the oxidation inhibitor that takes by weighing is added in the stirrer of preparing burden at a high speed, mix, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, and mixing time is 3-5 min, gets a Preblend.
7. described highly heat conductive polyphenylene sulfide material preparation method according to claim 1 is characterized in that, in the described step (1), adopts water-cooled to cool off, and adopts hot blast to carry out drying.
8. each described highly heat conductive polyphenylene sulfide material preparation method is characterized in that according to claim 1-7, in the described step (2), adopts a kind of metallic membrane for preparing in copper, silver, aluminium, nickel, the zirconium.
9. described highly heat conductive polyphenylene sulfide material preparation method according to claim 1, it is characterized in that, in the described step (3), the high-crystallinity polyphenylene sulfide that takes by weighing, high heat conducting fiber, crystalline thermoplastic resin are added in the stirrer of preparing burden at a high speed, mix, get secondary Preblend, wherein, the rotating speed of stirrer of preparing burden at a high speed is 480-960 r/min, and mixing time is 2-4 min.
10. the material of arbitrary described highly heat conductive polyphenylene sulfide material preparation method preparation according to claim 1-9.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104552970A (en) * | 2013-10-25 | 2015-04-29 | 中国石油化工股份有限公司 | Polymer composite fiber containing superfine metal fibers and preparation method of polymer composite fiber |
| CN106832760A (en) * | 2017-01-13 | 2017-06-13 | 江门市德众泰工程塑胶科技有限公司 | A kind of mobile phone Kato composite and its preparation method and application |
| CN106928642A (en) * | 2017-04-13 | 2017-07-07 | 上海博息电子科技有限公司 | The structural member and mobile terminal of mobile terminal |
| CN106977922A (en) * | 2017-04-17 | 2017-07-25 | 东莞市百励兴新材料有限公司 | A kind of highly heat conductive polyphenylene sulfide composite material and preparation method thereof |
| CN107151444A (en) * | 2017-07-12 | 2017-09-12 | 合肥东恒锐电子科技有限公司 | A kind of preparation method of electronic product casing material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4211687A (en) * | 1977-07-27 | 1980-07-08 | Hooker Chemicals & Plastics Corp. | Polymer blends with improved flame retardance |
| CN101407637A (en) * | 2008-11-21 | 2009-04-15 | 华东理工大学 | Fiber reinforced composite material and preparation thereof |
| CN101993602A (en) * | 2009-08-17 | 2011-03-30 | 莱尔德电子材料(深圳)有限公司 | Highly thermally-conductive moldable thermoplastic composites and compositions |
| JP2011084827A (en) * | 2009-10-14 | 2011-04-28 | Toray Ind Inc | Core-sheath type conjugate fiber |
| CN102174254A (en) * | 2010-12-27 | 2011-09-07 | 东莞劲胜精密组件股份有限公司 | Highly heat-conducting insulation engineering plastic and preparation method thereof |
| CN102876040A (en) * | 2012-10-08 | 2013-01-16 | 合肥杰事杰新材料股份有限公司 | Polyphenylene sulfide composite material and preparation method thereof |
-
2013
- 2013-07-11 CN CN201310289893.1A patent/CN103319893B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4211687A (en) * | 1977-07-27 | 1980-07-08 | Hooker Chemicals & Plastics Corp. | Polymer blends with improved flame retardance |
| CN101407637A (en) * | 2008-11-21 | 2009-04-15 | 华东理工大学 | Fiber reinforced composite material and preparation thereof |
| CN101993602A (en) * | 2009-08-17 | 2011-03-30 | 莱尔德电子材料(深圳)有限公司 | Highly thermally-conductive moldable thermoplastic composites and compositions |
| JP2011084827A (en) * | 2009-10-14 | 2011-04-28 | Toray Ind Inc | Core-sheath type conjugate fiber |
| CN102174254A (en) * | 2010-12-27 | 2011-09-07 | 东莞劲胜精密组件股份有限公司 | Highly heat-conducting insulation engineering plastic and preparation method thereof |
| CN102876040A (en) * | 2012-10-08 | 2013-01-16 | 合肥杰事杰新材料股份有限公司 | Polyphenylene sulfide composite material and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104552970A (en) * | 2013-10-25 | 2015-04-29 | 中国石油化工股份有限公司 | Polymer composite fiber containing superfine metal fibers and preparation method of polymer composite fiber |
| CN104552970B (en) * | 2013-10-25 | 2018-11-30 | 中国石油化工股份有限公司 | A kind of polymer composite fibrous preparation method and its preparation containing ultrafine metal fibers it is polymer composite fibrous |
| CN106832760A (en) * | 2017-01-13 | 2017-06-13 | 江门市德众泰工程塑胶科技有限公司 | A kind of mobile phone Kato composite and its preparation method and application |
| CN106832760B (en) * | 2017-01-13 | 2018-10-12 | 江门市德众泰工程塑胶科技有限公司 | A kind of mobile phone Kato composite material and preparation method and application |
| CN106928642A (en) * | 2017-04-13 | 2017-07-07 | 上海博息电子科技有限公司 | The structural member and mobile terminal of mobile terminal |
| CN106977922A (en) * | 2017-04-17 | 2017-07-25 | 东莞市百励兴新材料有限公司 | A kind of highly heat conductive polyphenylene sulfide composite material and preparation method thereof |
| CN107151444A (en) * | 2017-07-12 | 2017-09-12 | 合肥东恒锐电子科技有限公司 | A kind of preparation method of electronic product casing material |
| CN114045030A (en) * | 2021-11-25 | 2022-02-15 | 深圳烯湾科技有限公司 | Thermoplastic heat-conducting insulating composite material and preparation method thereof |
| CN114045030B (en) * | 2021-11-25 | 2023-09-15 | 深圳烯湾科技有限公司 | Thermoplastic heat-conducting insulating composite material and preparation method thereof |
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Address after: 621000 Hebei Pingwu Industrial Park, Sichuan, Mianyang Patentee after: SICHUAN COREMER CO., LTD. Address before: 621000 Hebei Pingwu Industrial Park, Sichuan, Mianyang Patentee before: Sichuan Coremer Materials Co., Ltd. |