CN102746623B - Preparation method for insulating heat conduction material - Google Patents

Preparation method for insulating heat conduction material Download PDF

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Publication number
CN102746623B
CN102746623B CN201110377355.9A CN201110377355A CN102746623B CN 102746623 B CN102746623 B CN 102746623B CN 201110377355 A CN201110377355 A CN 201110377355A CN 102746623 B CN102746623 B CN 102746623B
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China
Prior art keywords
temperature
screw extruder
twin
heat conduction
zones
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Expired - Fee Related
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CN201110377355.9A
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Chinese (zh)
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CN102746623A (en
Inventor
张明
欧正清
支长勇
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NANJING HONGRUI PLASTIC PRODUCTS CO Ltd
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NANJING HONGRUI PLASTIC PRODUCTS CO Ltd
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Priority to CN201110377355.9A priority Critical patent/CN102746623B/en
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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
    • 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
    • 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
    • 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
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • 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
    • 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
    • B29C2948/92885—Screw or gear
    • 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
    • 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
    • B29C2948/92904—Die; Nozzle zone

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a preparation method for an insulating heat conduction material. The preparation method comprises: uniformly mixing polybutylene terephthalate, metal fibers, an inorganic heat conduction filler, a toughening agent, a coupling agent, and a lubricant; and carrying out melt blending in a twin-screw extruder while adding glass fibers, and carrying out extrusion pelletizing. Process conditions of the extruder are that: the temperature of the zones 1-2 of the twin-screw extruder is 190-220 DEG C, the temperature of the zones 3-4 of the twin-screw extruder is 230-250 DEG C, the temperature of the zones 5-6 of the twin-screw extruder is 230-250 DEG C, the temperature of the zones 7-8 of the twin-screw extruder is 240-270 DEG C, the temperature of the extruder head is 230-250 DEG C, and the rotation speed of the screw is 150-350 rotations per minute. The raw materials comprise, by weight, 40-55% of the polybutylene terephthalate, 5-15% of the metal fibers, 25-45% of the inorganic heat conduction filler, 5-10% of the toughening agent, 0.1-1% of the coupling agent, and 0.1-0.5% of the lubricant. With the material prepared by the method of the present invention, the filling amount can be effectively reduced, the good insulation can be maintained well, and the high notched impact strength is provided.

Description

A kind of preparation method of insulating heat-conduction material
Technical field
The present invention relates to a kind of preparation method of insulating heat-conduction material, can be applicable to the fields such as electronic apparatus, heat exchange engineering, friction materials, belong to technical field of polymer materials.
Background technology
Along with industrial production and scientific and technical development, in fields such as heat exchange engineering, electromagnetic shielding, electric, friction materialss, insulating heat-conductive macromolecular material, due to the characteristic that it is corrosion-resistant, insulate, easily process, has more and more substituted thermal conductive metallic material and thermal conductive ceramic material.
In recent years, employing matrix plastic is the general-purpose plastics such as polypropylene, polyvinyl chloride, and heat conductive filler is mainly metal powder, steel fiber, graphite, carbon black, carbon fiber etc., good heat conductivity, but also make the decreasing insulating of material even become electro-conductive material.
At present, people utilize dielectric metal oxide and other compound filled polymers, have tentatively solved this problem.Insulated type conductive filler material mainly comprises BeO, MgO, Al 2o 3, NiO, AlN, BN, SiC, B 4c 3deng, but there is common problem in these fillers, and the loading level of filler is huge, and more than at least 60%, injection molding difficulty, the mechanical property of materials after compound is toughness extreme difference especially, and its practicality is had a greatly reduced quality.
As Chinese patent CN200510101700.0 discloses, a kind ofly take macrobead heat conductive filler and be the insulating and heat-conducting plastics of main injection moulding, its loading level is minimum is 71%(parts by weight), mostly be 86%(parts by weight most), notched Izod impact strength is only 3.3KJ/m 2; And for example Chinese patent CN200810025883.6 discloses that a kind of to take heat conductive filler and roving glass fiber be the insulating and heat-conducting plastics of main high mechanical strength, and its composite filled amount is minimum is 60%, mostly is 75% most, and notched Izod impact strength also only has 4.3～5.2KJ/m 2; For another example Chinese patent CN201010019386.2 discloses the coated heat conductive filler of a kind of resol insulating and heat-conducting plastics compound with matrix plastic again, and its loading level is also 75%, and notched Izod impact strength only has 2.9～4.1KJ/m 2.
Summary of the invention
The object of the invention is the shortcoming of many, the difficult processing of the filling existing for insulation conductive plastics, easy brittle failure, proposes a kind of compound method of preparing insulating and heat-conducting plastics of electro-conductive fiber and non-conducting filler.The a small amount of electro-conductive fiber of the method utilization forms disjunct skeleton structure in plastic substrate, filling appropriate non-conducting filler, in material, form interconnection can heat conduction nonconducting network structure, effectively reduce loading level, minimum needs fill 40%, keep good insulating heat-conductive simultaneously.And add a small amount of toughner, make matrix material there is higher notched Izod impact strength.
Concrete technical scheme of the present invention is as follows:
Polybutylene terephthalate, steel fiber, inorganic heat conductive filler, toughner, coupling agent and mix lubricant is even, melt blending in twin screw extruder, extruding pelletization; Forcing machine processing condition are: twin screw extruder 1-2 district temperature is 190-220 ℃, 3-4 district temperature is 230-250 ℃, and 5-6 district temperature is 230-250 ℃, and 7-8 district temperature is 240-270 ℃, head temperature is 230-250 ℃, and screw speed is 150-350 rev/min; The weight consumption of above-mentioned each raw material is:
Above-mentioned polybutylene terephthalate (PBT) is the polycondensate of terephthalic acid and butyleneglycol, and this is well-known in the art, can select the different trades mark according to purposes.
Above-mentioned steel fiber is stainless steel short fiber, and filament diameter is preferably at 1～40 μ m, its reason be filament diameter as being less than 1 μ m, to add man-hour easily broken, be difficult for forming a kind of insulating heat-conductive strutting system; Filament diameter is as being greater than 40 μ m, and the final material surface making is coarse, and larger to production unit wearing and tearing.
Due to aluminium sesquioxide (Al 2o 3) low price, good insulating, therefore above-mentioned heat conduction inorganic filler is selected aluminium sesquioxide (Al 2o 3).Meanwhile, due to aluminium sesquioxide (Al 2o 3) microtexture be hexahedron, stacking volume is larger, can form comparatively intensive network structure with lower addition.Its fineness is talked about lower than 80 objects, and particle is excessively thick, and the material surface making is coarse; Fineness is talked about higher than 325 objects, and particle is meticulous, can cause loading level to strengthen, and therefore, its fineness is for to be advisable with 80～325 orders.
The terpolymer EP rubber (EPDM-g-MAH) of the preferred maleic anhydride graft of above-mentioned toughner or octene ethylene copolymer (POE-g-MAH), its melting index is 0.5-10g/10min, its reason is to exceed this scope can cause processing difficulties; Percentage of grafting is 0.3%-1.5%, and its reason is best in this scope intrinsic toughening effect, and too low toughening effect is not obvious, and too high material has obvious irritating smell
Above-mentioned coupling agent is γ-aminopropyl triethoxysilane; Lubricant is calcium stearate or N, N '-ethylenebisstearamide.
The insulating heat-conduction material that adopts the present invention to make, has reduced the addition of heat conductive filler, and minimum needs fill 40%, keep good insulating heat-conductive simultaneously.By adding a small amount of toughner, make matrix material there is higher notched Izod impact strength, be with a wide range of applications.
Embodiment
Following examples are in order to further explanation the present invention, but the present invention is not only limited to these embodiment.
Embodiment 1,2,3,4 and comparative example 1,2 are in Table 1.
The polybutylene terephthalate of listed formula ratio in table 1, steel fiber, heat conduction inorganic filler, toughner, coupling agent and lubricant are mixed in high-speed mixer to melt blending in twin screw extruder, extruding pelletization.Forcing machine processing condition are: twin screw extruder 1-2 district temperature is 190-220 ℃, 3-4 district temperature is 230-250 ℃, and 5-6 district temperature is 230-250 ℃, and 7-8 district temperature is 240-270 ℃, head temperature is 230-250 ℃, and screw speed is 150-350 rev/min.The performance of material is in Table 2.
Table 1:
Table 2:

Claims (1)

1. a preparation method for insulating heat-conduction material, it is characterized in that polybutylene terephthalate, steel fiber, inorganic heat conductive filler, toughner, coupling agent and mix lubricant even, melt blending in twin screw extruder, extruding pelletization; Forcing machine processing condition are: twin screw extruder 1-2 district temperature is 190-220 ℃, 3-4 district temperature is 230-250 ℃, and 5-6 district temperature is 230-250 ℃, and 7-8 district temperature is 240-270 ℃, head temperature is 230-250 ℃, and screw speed is 150-350 rev/min; The weight consumption of above-mentioned each raw material is:
Above-mentioned steel fiber is stainless steel short fiber, and filament diameter is at 1～40 μ m; Heat conduction inorganic filler is aluminium sesquioxide (Al 2o 3), fineness is 80～325 orders; Toughner is terpolymer EP rubber (EPDM-g-MAH) or the octene ethylene copolymer (POE-g-MAH) of maleic anhydride graft, and its melting index is 0.5-10g/10min, and percentage of grafting is 0.3%-1.5%; Coupling agent is γ-aminopropyl triethoxysilane; Lubricant is calcium stearate or N, N '-ethylenebisstearamide.
CN201110377355.9A 2011-11-24 2011-11-24 Preparation method for insulating heat conduction material Expired - Fee Related CN102746623B (en)

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Families Citing this family (10)

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Publication number Priority date Publication date Assignee Title
JP6439244B2 (en) * 2013-05-30 2018-12-19 オイレス工業株式会社 Seismic isolation device
CN103467931B (en) * 2013-08-07 2016-01-13 上海日之升新技术发展有限公司 Continuous long aluminum fiber strengthens PBT mixture and preparation method thereof
CN104015327B (en) * 2014-05-09 2019-09-13 东莞市兆科电子材料科技有限公司 A kind of production method and production line of metal and the compound Heat Conduction Material of plastics
CN104015323A (en) * 2014-05-09 2014-09-03 东莞市兆科电子材料科技有限公司 Production method and production line of heat conduction plastics
US10400102B2 (en) 2014-06-09 2019-09-03 SABIC Global Technologies B.V Thermal conductive compositions having good impact performance
KR101806741B1 (en) * 2016-10-25 2017-12-08 현대자동차주식회사 Balancing weight with excellent extrudability
CN107177176B (en) * 2017-07-11 2019-03-19 无锡赢同新材料科技有限公司 With thermally conductive and conducting function high-modulus PBT composition and preparation method thereof
US11466130B2 (en) * 2017-11-20 2022-10-11 Ticona Llc Fiber-reinforced polymer composition for use in an electronic module
CN108770096A (en) * 2018-08-20 2018-11-06 深圳市同益高新电子科技有限公司 A kind of preparation process of heating film
CN114276789B (en) * 2021-12-31 2023-12-08 北京中石伟业科技股份有限公司 High-thixotropic silicon-based heat-conducting gel and preparation method thereof

Citations (2)

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Publication number Priority date Publication date Assignee Title
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
CN102181133A (en) * 2011-01-27 2011-09-14 上海锦湖日丽塑料有限公司 Metal fiber reinforced polybutylene terephthalate (PBT) resin and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102181133A (en) * 2011-01-27 2011-09-14 上海锦湖日丽塑料有限公司 Metal fiber reinforced polybutylene terephthalate (PBT) resin and preparation method thereof

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