CN106243620B - A kind of polyether-ether-ketone heat-conductive composite material and its preparation method and application - Google Patents
A kind of polyether-ether-ketone heat-conductive composite material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of polyether-ether-ketone heat-conductive composite materials and its preparation method and application.The recipe ingredient of the heat-conductive composite material is by weight：100 parts of polyether-ether-ketone, 10~30 parts of heat filling, 0.3~1.0 part of antioxidant；PEEK heat-conductive composite material is obtained using the method for compression molding, solves polyether-ether-ketone under high temperature long-time use condition, the thermally conductive problem of composite material, so that the heat resistance of polyether-ether-ketone be made to improve 10~20 DEG C.Has many advantages, such as antistatic, high temperature resistant, corrosion-resistant, and processing technology is simple.This kind of polyether-ether-ketone composite material thermal coefficient significantly improves, it can be used for producing the thermally conductive associated materials such as heat conductive insulating plate, heat-conduction circuit board, heat exchange material, anti-friction bearing and petrochemical industry, it can satisfy in engineering field and required under harsh conditions, especially requirement under the conditions of high-temperature heat-conductive, improves its application range conscientiously.
Description
Technical field
The present invention relates to a kind of polyether-ether-ketone heat-conductive composite materials and its preparation method and application, belong to high molecular material and add
Work field.
Background technique
Traditional Heat Conduction Material is mostly metal and metal oxide and other nonmetallic materials.Common high molecular materials, such as
The heat conductivity of polyolefin, polycarbonate, polyester etc. is poor, belongs to the non-conductor of heat, in answering for the occasion that needs to conduct heat and radiate
With being very limited.In order to improve the heating conduction of high molecular material, the metal or inorganic thermally conductive of high-termal conductivity is generallyd use
Filler is blended with high molecular material.The thermal conductivity of blended compound material can achieve tens times even 100 of base resin
Times, and have the advantages that not available for many conventional thermal conductive materials, such as：For needing thermally conductive and electrical isolation occasion：According to
Need to adjust the thermal coefficient of material；It is formed using the method for compression molding or injection molding, easy to process, high production efficiency,
Production cost is low.Heat-conducting plastic using very extensive, it can substitute metal, metal alloy and ceramic material as heat exchange
Device can also be applied in electronic and electrical industry, such as circuit board, electric appliance casing.
But current most polymers base heat-conductive composite material is limited to the performance requirement of polymer, be unable to satisfy industry,
Used under certain harsh conditions such as military project, aerospace and 200 DEG C or more hot conditions under requirement.
Summary of the invention
It is lower using temperature that the purpose of the present invention is the polymer matrix Heat Conduction Materials for the prior art, uses temperature change
The disadvantages of range is smaller and provide a kind of polyether-ether-ketone heat-conductive composite material and its preparation method and application, while making traditional poly-
The long-term use temperature of ether ether ketone improves 10~20 DEG C.Its main feature is that being made in short term at 300 DEG C using that can be used for a long time at 250 DEG C
Semi-crystalline state aromatic polyether-ether ketone resin is matrix, and the filler by adding different heating conductions prepares composite material.?
Combine polyether-ether-ketone excellent high temperature resistance, high intensity, high-dimensional stability and it is corrosion-resistant the features such as on the basis of impart material and lead
Hot property.It is small using range of temperature to solve traditional polymer matrix Heat Conduction Material, is unable to satisfy the harsh conditions such as high temperature
The problems such as lower use.The material can satisfy requirement under the harsh conditions such as high temperature, and use temperature range is wide, while also have
The features such as high intensity, high-dimensional stability.
In order to achieve the above objectives, technical scheme is as follows:A kind of polyether-ether-ketone heat-conductive composite material, this is thermally conductive multiple
The recipe ingredient of condensation material is by weight：100 parts of polyether-ether-ketone, 10~30 parts of heat filling, 0.3~1.0 part of antioxidant；
The heat filling is any one or above-mentioned filler in copper powder, aluminum oxide, aluminium nitride or short carbon fiber
Mixed fillers；
The antioxidant is antioxidant 1010, any one in antioxidant 168.
Preferably, the recipe ingredient of the heat-conductive composite material is by weight：100 parts of polyether-ether-ketone, 8~18 parts of copper powder,
4~9 parts of short carbon fiber, 0.3~0.5 part of antioxidant.
Second purpose of the invention be the preparation method of above-mentioned polyether-ether-ketone heat-conductive composite material is claimed, including with
Lower step：
S1 is dry by polyether-ether-ketone；
After S2 mixes polyether-ether-ketone, heat filling, antioxidant of the step S1 after dry, in high-speed stirred in blender
Mixing；
Step S2 resulting materials are put into mould cavity by S3, and pressurize 10MPa, pressure maintaining 5min, and modeling is melted in heating furnace
After change, pressurization 10MPa forms material, after pressure maintaining 20min, cools down with mold, demoulds；
S4 will demould material heat preservation after cooling, and product is made.
Preferably, step S1 condition is：Polyether-ether-ketone is 2~4 hours dry at a temperature of 140~160 DEG C.
Preferably, in step S2, blender speed is 2000rpm, and high-speed stirred mixes 8~10min.
Preferably, step S3 is specially：Material after stirring is put into mould cavity, pressurize 10MPa, pressure maintaining 5min it
Afterwards, it is put into the heating furnace that temperature is 380~390 DEG C, after heating 1~2 hour fusion plastification, pressurization 10MPa forms material,
After pressure maintaining 20min, when being cooled to 30 DEG C with mold, demoulding.
Preferably, heat-retaining condition is：1 hour is kept the temperature at a temperature of 250 DEG C.
Another object of the present invention is that the application of above-mentioned polyether-ether-ketone heat-conductive composite material, i.e. temperature change is claimed
The fields such as the biggish thermally conductive field of range and friction bearing, are used to prepare thermally conductive, the heat sink used under the harsh conditions such as high temperature.
The material that heat filling, which refers to, itself has high thermal conductivity and its heating conduction can be improved into certain matrix for filling
Material.Currently, common heat filling can be mainly divided into metal and inorganic filler two major classes.Heat-conducting polymer material is exactly based on
Addition heat filling just has excellent heating conduction, thus heat filling is the master for influencing the final heating conduction of high molecular material
Want factor.Cu powder is a kind of filler with high thermal conductivity, and staple fiber (SCF) has certain draw ratio, and thermal conductivity is high, can be very
Good plays the role of bridge joint, is conducive to the formation of heat conduction network.Aluminium nitride and antioxidant compounding, have certain synergistic effect,
The heating conduction of composite material can be effectively improved, and can improve PEEK hot procedure thermal stability and product size it is steady
It is qualitative.
It is improved in technique of the invention, using secondary pressurized, will release what material generated during heating
Gas releases stress, the compactness of product, the stability of size, crystallinity can be improved, and improve the mechanical property of product
Energy.
Compared with prior art, the beneficial effects of the invention are as follows：It is thermally conductive compound that PEEK is obtained using the method for compression molding
Material solves polyether-ether-ketone under high temperature long-time use condition, the thermally conductive problem of composite material, to make polyether-ether-ketone
Heat resistance improves 10~20 DEG C.Has many advantages, such as antistatic, high temperature resistant, corrosion-resistant, and processing technology is simple.This kind of polyethers ether
Ketone thermal conductivity of composite materials significantly improves, and can be used for producing heat conductive insulating plate, heat-conduction circuit board, heat exchange material, wear-resisting shaft
Hold with the thermally conductive associated materials such as petrochemical industry, can satisfy in engineering field and required under harsh conditions, especially led in high temperature
Requirement under heat condition improves its application range conscientiously.
Detailed description of the invention
Fig. 1 is the polyetheretherketonematerials materials microscopic appearance figure of comparison example of the present invention preparation；
Fig. 2 is polyether-ether-ketone/copper powder heat-conductive composite material microscopic appearance figure prepared by present example 3；
Fig. 3 is polyether-ether-ketone/copper powder heat-conductive composite material EDS photo prepared by present example 3；
Fig. 4 is polyether-ether-ketone/copper powder/short carbon fiber material microscopic appearance figure prepared by present example 4.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.In following embodiments unless otherwise specified, used experimental method is conventional method, used
Material, reagent etc. can chemically company be bought.Wherein the density of polyether-ether-ketone is 1.32g/cm3, copper powder size 5um, nitrogen
Change aluminum shot diameter is 25um, alumina particle 500nm.
Embodiment 1
100 parts of raw material polyether-ether-ketone are taken, 10 parts of copper powder, 0.3 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 4 hours dry at a temperature of 140 DEG C；
(b) it after the polyether-ether-ketone, copper powder, antioxidant mixing after taking step (a) dry, is put into blender, is rotating
High-speed stirred mixes 8min under the revolving speed that speed is 2000rpm；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 380 DEG C, after heating melting in 2 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with mould
When tool is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Embodiment 2
100 parts of raw material polyether-ether-ketone are taken, 30 parts of copper powder, 1 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 3 hours dry at a temperature of 150 DEG C；
(b) it after the polyether-ether-ketone, copper powder, antioxidant mixing after taking step (a) dry, is put into blender, is rotating
High-speed stirred mixes 10min under the revolving speed that speed is 2000rpm；
(c) mixed powder after step (b) stirring is put into mould cavity, pressurize 10MPa, after pressure maintaining 5min,
It is put into the heating furnace that temperature is 390 DEG C, after heating melting in 1 hour, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Embodiment 3
100 parts of raw material polyether-ether-ketone are taken, 15 parts of copper powder, 0.5 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 2 hours dry at a temperature of 160 DEG C；
(b) it after the polyether-ether-ketone, copper powder, antioxidant mixing after taking step (a) dry, is put into blender, is rotating
High-speed stirred mixes 10min under the revolving speed that speed is 2000rpm；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 385 DEG C, after heating melting in 1.5 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Embodiment 4
100 parts of raw material polyether-ether-ketone are taken, 10 parts of copper powder, 5 parts of short carbon fiber, 0.5 part of antioxidant, is made in the steps below
It is standby:
(a) polyether-ether-ketone is 3 hours dry at a temperature of 150 DEG C；
(b) after the polyether-ether-ketone, copper powder, short carbon fiber, antioxidant mixing after taking step (a) dry, it is put into blender
Interior, in the case where rotation speed is the revolving speed of 2000rpm, high-speed stirred mixes 10min；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 380 DEG C, after heating melting in 1.5 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Embodiment 5
100 parts of raw material polyether-ether-ketone are taken, 12 parts of aluminium nitride, 0.5 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 3 hours dry at a temperature of 150 DEG C；
(b) it after the polyether-ether-ketone, aluminium nitride, antioxidant mixing after taking step (a) dry, is put into blender, is revolving
High-speed stirred mixes 10min under the revolving speed that rotary speed is 2000rpm；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 380 DEG C, after heating melting in 1.5 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Embodiment 6
100 parts of raw material polyether-ether-ketone are taken, 12 parts of aluminium oxide, 0.5 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 3 hours dry at a temperature of 150 DEG C；
(b) it after the polyether-ether-ketone, aluminium oxide, antioxidant mixing after taking step (a) dry, is put into blender, is revolving
High-speed stirred mixes 10min under the revolving speed that rotary speed is 2000rpm；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 380 DEG C, after heating melting in 1.5 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Comparative example
100 parts of raw material polyether-ether-ketone are taken, 0.5 part of antioxidant, is prepared according to the following steps:
(a) polyether-ether-ketone is 3 hours dry at a temperature of 150 DEG C；
(b) it after the polyether-ether-ketone, antioxidant mixing after going step (a) dry, is put into blender, is in rotation speed
High-speed stirred mixes 10min under the revolving speed of 2000rpm；
(c) powder after being stirred step (b) is put into mould cavity, and pressurize 10MPa, after pressure maintaining 5min, is put
Enter in the heating furnace that temperature is 380 DEG C, after heating melting in 1.5 hours, pressurization 10MPa is pressed and molded, after pressure maintaining 20min, with
When mold is cooled to 30 DEG C, demoulding；
(d) step (c) is demoulded into moulding material after cooling and keeps the temperature 1 hour at a temperature of 250 DEG C, product is made.
Table 1 show the testing partial performances result of embodiment 3~6 and comparison example.
The performance of the polyether-ether-ketone heat-conductive composite material of the invention of table 1
From the data in table 1, it can be seen that the thermal coefficient for the heat-conductive composite material that the present invention obtains significantly improves, mechanical property is excellent
It is different.
Claims (3)
1. a kind of preparation method of polyether-ether-ketone heat-conductive composite material, which is characterized in that the recipe ingredient of the heat-conductive composite material
By weight：100 parts of polyether-ether-ketone, 10~30 parts of heat filling, 0.3~1.0 part of antioxidant；
The heat filling is the mixed of any one or the above-mentioned filler in copper powder, aluminum oxide, aluminium nitride or short carbon fiber
Close filler；Wherein the density of polyether-ether-ketone is 1.32g/cm3, copper powder size 5um, aluminium nitride partial size is 25um, aoxidizes aluminum shot
Diameter is 500nm；
The antioxidant is one of antioxidant 1010, antioxidant 168；
Include the following steps：
S1 is 2~4 hours dry at a temperature of 140~160 DEG C by polyether-ether-ketone；
It is mixed in high-speed stirred in blender after S2 mixes polyether-ether-ketone, heat filling, antioxidant of the step S1 after dry
It closes, blender speed is 2000rpm, and high-speed stirred mixes 8~10min；
Material after stirring is put into mould cavity by S3, and pressurize 10MPa, and after pressure maintaining 5min, being put into temperature is 380~390
DEG C heating furnace in, heat 1~2 hour fusion plastification after, pressurization 10MPa form material, after pressure maintaining 20min, with mold
When being cooled to 30 DEG C, demoulding；
S4 will demould material after cooling and keep the temperature heat preservation in 1 hour at a temperature of 250 DEG C, and product is made.
2. polyether-ether-ketone heat-conductive composite material preparation method according to claim 1, which is characterized in that the thermally conductive composite wood
The recipe ingredient of material is by weight：100 parts of polyether-ether-ketone, 8~18 parts of copper powder, 4~9 parts of short carbon fiber, antioxidant 0.3~
0.5 part.
3. a kind of application of the polyether-ether-ketone heat-conductive composite material of method preparation as described in claim 1, which is characterized in that be used for
Prepare thermally conductive, the heat sink used under high temperature harsh conditions.
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| CN107459770B (en) * | 2017-08-16 | 2020-03-24 | 宜宾天原集团股份有限公司 | High-thermal-conductivity polyether-ether-ketone composite material and preparation method thereof |
| CN110762122A (en) * | 2018-07-27 | 2020-02-07 | 哈尔滨电机厂有限责任公司 | Hot die pressing molding process for polyether-ether-ketone composite material thrust tile of pumped storage unit |
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| CN109438916A (en) * | 2018-10-25 | 2019-03-08 | 宜宾天原集团股份有限公司 | Heat-resisting antistatic polyether-ether-ketone composite material of one kind and preparation method thereof |
| CN110684512B (en) * | 2019-10-18 | 2021-04-20 | 吉林大学 | High-thermal-conductivity spherical sulfonated polyether ether ketone/graphite core-shell structure filler and preparation method thereof |
| CN110819065A (en) * | 2019-11-08 | 2020-02-21 | 太原理工大学 | Conductive wear-resistant light polyether ether ketone based composite material and preparation method thereof |
| CN113683861A (en) * | 2021-08-24 | 2021-11-23 | 江苏中科睿赛污染控制工程有限公司 | High-wear-resistance and high-thermal-conductivity composite material and preparation method and application thereof |
| CN113954471B (en) * | 2021-10-23 | 2022-07-05 | 佛山市达孚新材料有限公司 | Three-layer co-extrusion high-wear-resistance polyether-ether-ketone composite film and preparation method thereof |
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| CN102079864A (en) * | 2009-11-30 | 2011-06-01 | 比亚迪股份有限公司 | Insulating heat-conducting resin composition and plastic product thereof |
| CN101775213A (en) * | 2010-02-01 | 2010-07-14 | 黄晓峰 | High thermal conducting composite material and preparation method thereof |
| CN105778407A (en) * | 2016-04-25 | 2016-07-20 | 苏州亚科塑胶有限公司 | Polyether-ether-ketone heat conduction composite material and preparation method thereof |
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