CN106243620A - A kind of polyether-ether-ketone heat-conductive composite material and its production and use - Google Patents
A kind of polyether-ether-ketone heat-conductive composite material and its production and use Download PDFInfo
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Abstract
The present invention relates to a kind of polyether-ether-ketone heat-conductive composite material and its production and use.The recipe ingredient of this heat-conductive composite material is by weight: polyether-ether-ketone 100 parts, heat filling 10~30 parts, antioxidant 0.3~1.0 parts;The method using compression molding obtains PEEK heat-conductive composite material, solves polyether-ether-ketone under the conditions of high temperature uses for a long time, and a heat conduction difficult problem for composite, so that the thermostability of polyether-ether-ketone improves 10~20 DEG C.There is antistatic, high temperature resistant, corrosion-resistant, and the advantage such as processing technique is simple.This kind of polyether-ether-ketone composite material heat conductivity significantly improves, can be used for producing the heat conduction associated materials such as heat conductive insulating plate, heat-conduction circuit board, heat exchange material, anti-friction bearing and petrochemical industry, disclosure satisfy that requirement under harsh conditions in engineering field, under the conditions of high-temperature heat-conductive, especially use requirement, conscientiously improve its range of application.
Description
Technical field
The present invention relates to a kind of polyether-ether-ketone heat-conductive composite material and its production and use, belong to macromolecular material and add
Work field.
Background technology
Traditional Heat Conduction Material mostly is metal and metal-oxide and other nonmetallic materials.Common high molecular materials, as
The heat conductivity of polyolefin, Merlon, polyester etc. is poor, belong to heat non-conductor, need heat transfer and heat radiation occasion should
With being very limited.In order to improve the heat conductivility of macromolecular material, generally use the metal of high-termal conductivity or inorganic heat conduction
Filler is blended with macromolecular material.The thermal conductivity of blended compound material can reach tens times even 100 of base resin
Times, and there is the advantage not available for many conventional thermal conductive materials, such as: for needing the occasion of heat conduction and electric insulation: according to
Need to adjust the heat conductivity of material;Using compression molding or the method molding of injection mo(u)lding, easy to process, production efficiency is high,
Production cost is low.The application of heat-conducting plastic is quite varied, and it can be used as heat exchange with alternative metals, metal alloy and ceramic material
Device, it is also possible to apply in electric industry, such as circuit board, electric appliance casing etc..
But most polymers base heat-conductive composite material is limited to the performance requirement of polymer at present, it is impossible to satisfied industry,
Under some harsh conditions such as military project, Aero-Space use and 200 DEG C of high temperature above under the conditions of use requirement.
Summary of the invention
It is an object of the invention to use for the polymer base heat conducting material of prior art temperature relatively low, use variations in temperature
The shortcomings such as scope is less and a kind of polyether-ether-ketone heat-conductive composite material and its production and use is provided, make traditional poly-simultaneously
The life-time service temperature of ether ether ketone improves 10~20 DEG C.Being characterized in that employing can be at 250 DEG C of life-time service, at 300 DEG C, short-term makes
Semi-crystalline state aromatic polyether-ether ketone resin be matrix, prepare composite by adding the filler of different heat conductivility.?
Impart material on the basis of combining polyether-ether-ketone excellent high temperature resistance, high intensity, high-dimensional stability and the feature such as corrosion-resistant to lead
Hot property.Solving traditional polymer base heat conducting material uses range of temperature little, it is impossible to meet the harsh conditions such as high temperature
The problems such as lower use.This material disclosure satisfy that use requirement under the harsh conditions such as high temperature, uses temperature range wide, the most also has
The feature such as high intensity, high-dimensional stability.
For reaching above-mentioned purpose, technical scheme is as follows: a kind of polyether-ether-ketone heat-conductive composite material, and this heat conduction is multiple
The recipe ingredient of condensation material is by weight: polyether-ether-ketone 100 parts, heat filling 10~30 parts, antioxidant 0.3~1.0 parts;
Described heat filling is any one or above-mentioned filler in copper powder, aluminium sesquioxide, aluminium nitride or short carbon fiber
Mixed fillers;
Described antioxidant is any one in antioxidant 1010, antioxidant 168.
Preferably, the recipe ingredient of this heat-conductive composite material by weight: polyether-ether-ketone 100 parts, copper powder 8~18 parts,
Short carbon fiber 4~9 parts, antioxidant 0.3~0.5 part.
Second purpose of the present invention is the preparation method that above-mentioned polyether-ether-ketone heat-conductive composite material is claimed, including with
Lower step:
Polyether-ether-ketone is dried by S1;
After dried for step S1 polyether-ether-ketone, heat filling, antioxidant are mixed by S2, high-speed stirred in blender
Mixing;
Step S2 resulting materials is put into mould cavity by S3, and pressurize 10MPa, pressurize 5min, melts and mould in heating furnace
After change, pressurization 10MPa makes material molding, after pressurize 20min, lowers the temperature with mould, the demoulding;
Material after the demoulding is cooled down by S4 is incubated, and prepares product.
Preferably, step S1 condition is: be dried 2~4 hours at a temperature of 140~160 DEG C by polyether-ether-ketone.
Preferably, in step S2, blender speed is 2000rpm, high-speed stirred mixing 8~10min.
Preferably, step S3 particularly as follows: the material after stirring is put into mould cavity, pressurization 10MPa, pressurize 5min it
After, put in the heating furnace that temperature is 380~390 DEG C, after heating 1~2 hour fusion plastification, pressurization 10MPa makes material molding,
After pressurize 20min, when being cooled to 30 DEG C with mould, the demoulding.
Preferably, heat-retaining condition is: be incubated 1 hour 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. variations in temperature are claimed
The fields such as heat conduction field that scope is bigger and friction bearing, for preparing heat conduction, the heat sink used under the harsh conditions such as high temperature.
Heat filling refers to self have high thermal conductivity and fill the material that can improve its heat conductivility to certain matrix
Material.At present, common heat filling can be largely classified into metal and the big class of inorganic filler two.Heat-conducting polymer material is exactly based on
Add heat filling and just there is the heat conductivility of excellence, thus heat filling is the master affecting the final heat conductivility of macromolecular material
Want factor.Cu powder is a kind of filler with high thermal conductivity, and chopped fiber (SCF) has certain draw ratio, and thermal conductivity is high, can be very
Good bridge joint effect of playing, the beneficially formation of heat conduction network.Aluminium nitride and antioxidant compound, and have certain cooperative effect,
Can be effectively improved the heat conductivility of composite, and the size that can improve the heat stability of PEEK hot procedure and goods is steady
Qualitative.
Improved in the technique of the present invention, use secondary pressurized, will release what material produced during heating
Gas, releases stress, can improve the degree of compaction of goods, the stability of size, crystallinity, and improves the mechanical property of goods
Energy.
Compared with prior art, the invention has the beneficial effects as follows: use the method for compression molding to obtain PEEK heat conduction and be combined
Material, solves polyether-ether-ketone under the conditions of high temperature uses for a long time, a heat conduction difficult problem for composite, so that polyether-ether-ketone
Thermostability improves 10~20 DEG C.There is antistatic, high temperature resistant, corrosion-resistant, and the advantage such as processing technique 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 and the heat conduction associated materials such as petrochemical industry, it is possible to meet requirement under harsh conditions in engineering field, especially lead at high temperature
Use requirement under heat condition, conscientiously improve its range of application.
Accompanying drawing explanation
Fig. 1 is polyetheretherketonematerials materials microscopic appearance figure prepared by comparison example of the present invention;
Fig. 2 is the polyether-ether-ketone/copper powder heat-conductive composite material microscopic appearance figure of present example 3 preparation;
Fig. 3 is the EDS photo of the polyether-ether-ketone/copper powder heat-conductive composite material of present example 3 preparation;
Fig. 4 is the polyether-ether-ketone/copper powder/short carbon fiber material microscopic appearance figure of present example 4 preparation.
Detailed description of the invention
Following non-limiting example can make those of ordinary skill in the art that the present invention be more fully understood, but not with
Any mode limits the present invention.In following embodiment if no special instructions, the experimental technique used is conventional method, used
Material, reagent etc. all can chemically company be bought.Wherein the density of polyether-ether-ketone is 1.32g/cm3, copper powder size is 5um, nitrogen
Changing aluminum shot footpath is 25um, and alumina particle is 500nm.
Embodiment 1
Take raw material polyether-ether-ketone 100 parts, copper powder 10 parts, antioxidant 0.3 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 4 hours at a temperature of 140 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), copper powder, antioxidant mixing after, put into blender, rotating
Speed be 2000rpm rotating speed under high-speed stirred mixing 8min;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Entering in the heating furnace that temperature is 380 DEG C, heat 2 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with mould
When tool is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Embodiment 2
Take raw material polyether-ether-ketone 100 parts, copper powder 30 parts, antioxidant 1 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 3 hours at a temperature of 150 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), copper powder, antioxidant mixing after, put into blender, rotating
Speed be 2000rpm rotating speed under high-speed stirred mixing 10min;
C step (b) is stirred by () after, mould cavity put into by mixed powder, and pressurize 10MPa, after pressurize 5min,
Put in the heating furnace that temperature is 390 DEG C, heat 1 hour after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Embodiment 3
Take raw material polyether-ether-ketone 100 parts, copper powder 15 parts, antioxidant 0.5 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 2 hours at a temperature of 160 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), copper powder, antioxidant mixing after, put into blender, rotating
Speed be 2000rpm rotating speed under high-speed stirred mixing 10min;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Enter in the heating furnace that temperature is 385 DEG C, heat 1.5 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Embodiment 4
Take raw material polyether-ether-ketone 100 parts, copper powder 10 parts, short carbon fiber 5 parts, antioxidant 0.5 part, make in the steps below
Standby:
A polyether-ether-ketone is dried 3 hours at a temperature of 150 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), copper powder, short carbon fiber, antioxidant mixing after, put into blender
In, high-speed stirred mixing 10min under the rotating speed that rotary speed is 2000rpm;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Enter in the heating furnace that temperature is 380 DEG C, heat 1.5 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Embodiment 5
Take raw material polyether-ether-ketone 100 parts, aluminium nitride 12 parts, antioxidant 0.5 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 3 hours at a temperature of 150 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), aluminium nitride, antioxidant mixing after, put into blender, in rotation
Rotary speed be 2000rpm rotating speed under high-speed stirred mixing 10min;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Enter in the heating furnace that temperature is 380 DEG C, heat 1.5 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Embodiment 6
Take raw material polyether-ether-ketone 100 parts, aluminium oxide 12 parts, antioxidant 0.5 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 3 hours at a temperature of 150 DEG C by ();
B () takes the dried polyether-ether-ketone of step (a), aluminium oxide, antioxidant mixing after, put into blender, in rotation
Rotary speed be 2000rpm rotating speed under high-speed stirred mixing 10min;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Enter in the heating furnace that temperature is 380 DEG C, heat 1.5 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Comparative example
Take raw material polyether-ether-ketone 100 parts, antioxidant 0.5 part, be prepared according to the following steps:
A polyether-ether-ketone is dried 3 hours at a temperature of 150 DEG C by ();
B () goes the mixing of the dried polyether-ether-ketone of step (a), antioxidant after, put into blender, in rotary speed be
High-speed stirred mixing 10min under the rotating speed of 2000rpm;
C step (b) is stirred mixed powder and puts into mould cavity by (), pressurize 10MPa, after pressurize 5min, puts
Enter in the heating furnace that temperature is 380 DEG C, heat 1.5 hours after melting, 10MPa compression molding of pressurizeing, after pressurize 20min, with
When mould is cooled to 30 DEG C, the demoulding;
Moulding material d step (c) demoulding is cooled down by () after is incubated 1 hour at a temperature of 250 DEG C, prepares product.
Table 1 show embodiment 3~6 and the testing partial performances result of comparison example.
The performance of the polyether-ether-ketone heat-conductive composite material of table 1 present invention
From the data in table 1, it can be seen that the heat conductivity of heat-conductive composite material that the present invention obtains significantly improves, mechanical property is excellent
Different.
Claims (8)
1. a polyether-ether-ketone heat-conductive composite material, it is characterised in that the recipe ingredient of this heat-conductive composite material by weight:
Polyether-ether-ketone 100 parts, heat filling 10~30 parts, antioxidant 0.3~1.0 parts;
Described heat filling is the mixed of any one or the above-mentioned filler in copper powder, aluminium sesquioxide, aluminium nitride or short carbon fiber
Close filler;
Described antioxidant is any one in antioxidant 1010, antioxidant 168.
Polyether-ether-ketone heat-conductive composite material the most according to claim 1, it is characterised in that the formula of this heat-conductive composite material
Composition by weight is: polyether-ether-ketone 100 parts, copper powder 8~18 parts, short carbon fiber 4~9 parts, antioxidant 0.3~0.5 part.
3. the preparation method of a polyether-ether-ketone heat-conductive composite material as claimed in claim 1, it is characterised in that include following
Step:
Polyether-ether-ketone is dried by S1;
S2 is by after dried for step S1 polyether-ether-ketone, heat filling, antioxidant mixing, and in blender, high-speed stirred is mixed
Close;
Step S2 resulting materials is put into mould cavity by S3, and pressurize 10MPa, pressurize 5min, in heating furnace after fusion plastification,
Pressurization 10MPa makes material molding, after pressurize 20min, lowers the temperature with mould, the demoulding;
Material after the demoulding is cooled down by S4 is incubated, and prepares product.
The preparation method of polyether-ether-ketone heat-conductive composite material the most according to claim 3, it is characterised in that step S1 condition
For: polyether-ether-ketone is dried 2~4 hours at a temperature of 140~160 DEG C.
The preparation method of polyether-ether-ketone heat-conductive composite material the most according to claim 3, it is characterised in that in step S2,
Blender speed is 2000rpm, high-speed stirred mixing 8~10min.
The preparation method of polyether-ether-ketone heat-conductive composite material the most according to claim 3, it is characterised in that step S3 is concrete
For: the material after stirring is put into mould cavity, and pressurize 10MPa, and after pressurize 5min, putting into temperature is 380~390 DEG C
In heating furnace, after heating 1~2 hour fusion plastification, pressurization 10MPa makes material molding, after pressurize 20min, lowers the temperature with mould
During to 30 DEG C, the demoulding.
The preparation method of polyether-ether-ketone heat-conductive composite material the most according to claim 3, it is characterised in that heat-retaining condition
It is: at a temperature of 250 DEG C, be incubated 1 hour.
8. the application of the polyether-ether-ketone heat-conductive composite material described in claim 1, it is characterised in that be used for preparing the harshnesses such as high temperature
Under the conditions of use heat conduction, heat sink.
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CN107459770A (en) * | 2017-08-16 | 2017-12-12 | 宜宾天原集团股份有限公司 | A kind of high-termal conductivity polyether-ether-ketone composite material and preparation method thereof |
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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 |
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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 |
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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 |
CN113954471A (en) * | 2021-10-23 | 2022-01-21 | 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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