CN107459770B - High-thermal-conductivity polyether-ether-ketone composite material and preparation method thereof - Google Patents
High-thermal-conductivity polyether-ether-ketone composite material and preparation method thereof Download PDFInfo
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- 239000004696 Poly ether ether ketone Substances 0.000 title claims abstract description 80
- 229920002530 polyetherether ketone Polymers 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920002748 Basalt fiber Polymers 0.000 claims abstract description 52
- 229910052582 BN Inorganic materials 0.000 claims abstract description 41
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 41
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 41
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 22
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 9
- 239000012778 molding material Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 5
- 229920006351 engineering plastic Polymers 0.000 abstract description 9
- 239000000945 filler Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- -1 ether ketone Chemical class 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 229920006260 polyaryletherketone Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- C08K3/34—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K7/04—Fibres or whiskers inorganic
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention relates to a special engineering plastic, and particularly discloses a high-thermal-conductivity polyether-ether-ketone composite material which is prepared from the following raw materials in parts by weight: 60-75 parts of polyether-ether-ketone, 5-10 parts of silicon carbide, 5-10 parts of boron nitride, 10-20 parts of basalt fiber and 0.5-1 part of antioxidant; the invention takes polyether-ether-ketone as a matrix and takes silicon carbide, boron nitride and basalt fiber as compound heat-conducting fillers; the silicon carbide and the boron nitride have high thermal conductivity, and the basalt fiber has a certain length-diameter ratio, so that the bridging effect can be well played, and the formation of a heat-conducting network is facilitated; the heat-conducting filler is compounded according to a certain proportion, so that the heat-conducting property of the composite material is synergistically improved; the composite material prepared by the invention has the characteristics of high thermal conductivity, high strength, high stability and the like, and can meet the use requirements under severe conditions such as high temperature and the like; because the cost of the basalt fiber is lower, the preparation cost of the heat-conducting polyether-ether-ketone composite material is reduced, and the heat-conducting polyether-ether-ketone composite material can be widely applied to industrialization.
Description
Technical Field
The invention relates to a special engineering plastic, in particular to a high-thermal-conductivity polyether-ether-ketone composite material.
Background
The special engineering plastics are also called high-performance engineering plastics, and are polymer materials which are mainly applied to the high-technology field, have excellent comprehensive performance and can be used at the temperature of more than 150 ℃ for a long time. The special engineering plastics have excellent characteristics of high specific strength, high heat resistance grade and the like, in recent years, research on the special engineering plastics is rapidly developed, and the industrialized special engineering plastics are various in types, and the main types are as follows: polyimide resins (PI), Polyaryletherketones (PAEK), and the like. Although the using amount of the special engineering plastic cannot be compared with that of the general plastic, the special engineering plastic has an irreplaceable status in the fields of aerospace, automobiles, electronics, nuclear energy and the like due to excellent using performance. Polyether ether ketone (PEEK) is the most typical material in polyarylether ketone (PAEK), has excellent comprehensive performance, and can obviously improve the performance of products after replacing other materials in many fields. Polyether-ether-ketone is gradually applied to the fields of aerospace, automobiles, energy sources and the like at present due to various excellent performances of mechanical property, wear resistance, chemical resistance, radiation resistance, high temperature resistance, flame retardance and the like. At present, the polyether-ether-ketone resin has poor heat conductivity and antistatic property due to lack of effective filler components, so that the wide application of the polyether-ether-ketone resin in the high-tech fields of electronic appliances, heat exchange engineering, chemical engineering and the like is limited. Therefore, the development of a high thermal conductivity polyetheretherketone composite material by selecting a proper filler is a problem to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity polyether-ether-ketone composite material which improves the thermal conductivity and the antistatic property of polyether-ether-ketone through a filler.
The technical scheme adopted by the invention for solving the technical problems is as follows: the high-thermal-conductivity polyether-ether-ketone composite material is prepared from the following raw materials in parts by weight: 60-75 parts of polyether-ether-ketone, 5-10 parts of silicon carbide, 5-10 parts of boron nitride, 10-20 parts of basalt fiber and 0.5-1 part of antioxidant.
Preferably, the particle size of the polyether-ether-ketone, the silicon carbide and the boron nitride is 15-20 μm.
Preferably, the basalt fibers are short fibers.
Preferably, the basalt fibers are short fibers with the diameter of 8-10 mm.
A preparation method of a high-thermal-conductivity polyether-ether-ketone composite material comprises the following steps:
(1) and (3) drying: providing raw materials of the high-thermal-conductivity polyetheretherketone composite material according to claim 1, and respectively drying polyetheretherketone, silicon carbide, boron nitride and basalt fiber at the temperature of 180-190 ℃ for 5-6 h;
(2) mixing: uniformly mixing the dried polyether-ether-ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant;
(3) and (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 2-3 MPa, maintaining the pressure for 10-20 min, heating to 380-400 ℃, keeping the temperature and maintaining the pressure for 3-4 h, then decompressing, cooling to 80-90 ℃, demolding, heating the demolded molding material to 270-280 ℃, and keeping the temperature for 2-3 h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Preferably, a high-speed mixer is selected for mixing in the step (2), and the rotating speed of the high-speed mixer is controlled to be 900-1000 r/min for mixing for 20-30 min.
The invention has the beneficial effects that: the invention takes polyether-ether-ketone as a matrix and takes silicon carbide, boron nitride and basalt fiber as compound heat-conducting fillers; the silicon carbide and the boron nitride have high thermal conductivity, and the basalt fiber has a certain length-diameter ratio, so that the bridging effect can be well played, and the formation of a heat-conducting network is facilitated. The heat-conducting filler is compounded according to a certain proportion, so that the heat-conducting property of the composite material is synergistically improved; the high-thermal-conductivity polyether-ether-ketone composite material prepared by the invention has the characteristics of high thermal conductivity, high strength, high stability and the like, and can meet the use requirements under severe conditions such as high temperature and the like; because the cost of the basalt fiber is lower, the preparation cost of the heat-conducting polyether-ether-ketone composite material is reduced, and the heat-conducting polyether-ether-ketone composite material can be widely applied to industrialization.
Drawings
FIG. 1 is a graph showing the effect of basalt fiber content on the thermal conductivity of PEEK composites.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
The high-thermal-conductivity polyether-ether-ketone composite material is prepared from the following raw materials in parts by weight: 60-75 parts of polyether-ether-ketone, 5-10 parts of silicon carbide, 5-10 parts of boron nitride, 10-20 parts of basalt fiber and 0.5-1 part of antioxidant. The particle sizes of the polyether-ether-ketone, the silicon carbide and the boron nitride are 15-20 mu m. The raw material particle size of 15-20 microns enables the purpose of homogeneity to be achieved in the preparation process, and a foundation is provided for the subsequent preparation of the high-thermal-conductivity polyether-ether-ketone composite material. The basalt fibers are short fibers with the diameter of 8-10 mm, so that raw materials can be mixed easily, a bridging effect can be well achieved, a heat conducting network can be formed easily, and the heat conducting performance of the polyether-ether-ketone composite material is improved. The density of the polyether-ether-ketone is 1.30g/cm3The antioxidant is selected from common antioxidants.
A preparation method of a high-thermal-conductivity polyether-ether-ketone composite material comprises the following steps:
(1) and (3) drying: providing raw materials of the high-thermal-conductivity polyetheretherketone composite material according to claim 1, and respectively drying polyetheretherketone, silicon carbide, boron nitride and basalt fiber at the temperature of 180-190 ℃ for 5-6h to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried polyether-ether-ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 20-30 min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 2-3 MPa, maintaining the pressure for 10-20 min, heating to 380-400 ℃, keeping the temperature and maintaining the pressure for 3-4 h, then decompressing, cooling to 80-90 ℃, demolding, heating the demolded molding material to 270-280 ℃, and keeping the temperature for 2-3 h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
According to the invention, the silicon carbide, the boron nitride and the basalt fiber are taken as heat-conducting fillers to play a synergistic role, so that the heat-conducting property of the PEEK is obviously improved. In order to research the influence of the content of basalt fibers on the thermal conductivity of the PEEK composite material, 70g of polyetheretherketone, 10g of silicon carbide, 5g of boron nitride and 1g of antioxidant are selected, and then 0g, 3g, 5g, 10g, 15g, 20g, 25g, 30g, 35g, 40g and 45g of basalt fibers are respectively added to prepare the PEEK composite material, and the thermal conductivity is tested, and the results are shown in FIG. 1 and can be seen: the thermal conductivity of the composite material is in an increasing trend along with the increase of the dosage of the basalt fiber, when the dosage of the basalt fiber is 10-20 g, the thermal conductivity is stably and maximally increased to 0.9W/m ℃, and when the dosage of the basalt fiber is further increased and exceeds 20g, the thermal conductivity is gradually reduced. Researches show that when the dosage of the basalt fiber is low, the basalt fiber, the silicon carbide and the boron nitride particles are respectively wrapped by PEEK resin and rarely contact with each other, so that the thermal conductivity of the composite material is low; with the increase of the dosage of the basalt fiber, the degree of the basalt fiber, the silicon carbide and the boron nitride particles which are wrapped by the PEEK resin is reduced, the capability of forming a heat conduction path in a system is enhanced, so that the heat conductivity of the composite material is increased, but after the dosage of the basalt fiber exceeds 20g, disorder is dispersed in the matrix, an effective heat conduction chain in the heat flow direction cannot be formed, the increase of the heat conductivity coefficient is limited, and the heat conductivity of the composite material has a gradual reduction trend. Therefore, when the amount of the basalt fibers in the high-thermal-conductivity polyether-ether-ketone composite material is 10-20 parts, the optimal excellent performance can be exerted, the bridging effect is fully achieved, isolated silicon carbide and boron nitride particles with high thermal conductivity are connected, and the thermal conductivity of the high-thermal-conductivity polyether-ether-ketone composite material is remarkably improved.
Example 1:
(1) and (3) drying: weighing 65 parts of polyether-ether-ketone, 10 parts of silicon carbide, 10 parts of boron nitride, 14 parts of 8-10 mm basalt fiber and 1 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at the temperature of 180 ℃ for 5 hours to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 30min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 3MPa, maintaining the pressure for 10min, heating to 390 ℃, keeping the temperature and the pressure for 3.5h, then decompressing, cooling to 80 ℃, demolding, heating the demolded molding material to 280 ℃, and keeping the temperature for 2h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Example 2:
(1) and (3) drying: weighing 69 parts of polyether-ether-ketone, 10 parts of silicon carbide, 10 parts of boron nitride, 10 parts of basalt fiber and 1 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at the temperature of 190 ℃ for 5.5 hours to enable the water content to be lower than 40 ppm; the particle sizes of the polyether-ether-ketone, the silicon carbide and the boron nitride are 15-20 mu m;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 20min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 2.5MPa, maintaining the pressure for 20min, heating to 380 ℃, keeping the temperature and the pressure for 4h, then decompressing, cooling to 90 ℃, demolding, heating the demolded molding material to 270 ℃, and keeping the temperature for 3h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Example 3:
(1) and (3) drying: weighing 74.5 parts of polyether-ether-ketone, 5 parts of silicon carbide, 10 parts of boron nitride, 10 parts of basalt fiber and 0.5 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at 185 ℃ for 6 hours to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 25min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 3MPa, maintaining the pressure for 10min, heating to 390 ℃, keeping the temperature and the pressure for 3.5h, then decompressing, cooling to 80 ℃, demolding, heating the demolded molding material to 280 ℃, and keeping the temperature for 2h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Example 4:
(1) and (3) drying: weighing 74 parts of polyether-ether-ketone, 8 parts of silicon carbide, 5 parts of boron nitride, 12 parts of basalt fiber and 1 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at the temperature of 180-190 ℃ for 5-6 hours to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 20-30 min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 2MPa, maintaining the pressure for 10min, heating to 400 ℃, keeping the temperature and the pressure for 3h, then decompressing, cooling to 80 ℃, demolding, heating the demolded molding material to 275 ℃, and keeping the temperature for 2.6h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Example 5:
(1) and (3) drying: weighing 66 parts of polyether-ether-ketone, 10 parts of silicon carbide, 8 parts of boron nitride, 15 parts of basalt fiber and 1 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at 185 ℃ for 6 hours to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 25min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 3MPa, maintaining the pressure for 10min, heating to 390 ℃, keeping the temperature and the pressure for 3.5h, then decompressing, cooling to 80 ℃, demolding, heating the demolded molding material to 280 ℃, and keeping the temperature for 2h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
Example 6:
(1) and (3) drying: weighing 69 parts of polyether-ether-ketone, 5 parts of silicon carbide, 5 parts of boron nitride, 20 parts of basalt fiber and 1 part of antioxidant, and respectively drying the polyether-ether-ketone, the silicon carbide, the boron nitride and the basalt fiber at the temperature of 180 ℃ for 5 hours to enable the water content to be lower than 40 ppm;
(2) mixing: and adding the dried ether ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant into a high-speed mixer, controlling the rotating speed of the high-speed mixer to be 900-1000 r/min, and mixing for 30min to mix uniformly.
(3) And (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 3MPa, maintaining the pressure for 10min, heating to 390 ℃, keeping the temperature and the pressure for 3.5h, then decompressing, cooling to 80 ℃, demolding, heating the demolded molding material to 280 ℃, and keeping the temperature for 2h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
The performance test of the high thermal conductivity polyetheretherketone composite materials obtained in examples 1 to 6 shows that the thermal conductivity of the high thermal conductivity polyetheretherketone composite material prepared by the invention is more than 0.86 and stable as shown in the following table; the flexural modulus reaches more than 22GPa, the IZOD impact strength is not less than 8.52kJ per square meter, and the high strength is expressed; the heat distortion temperature is above 379 ℃, and the heat resistance is strong.
TABLE 1 Properties of high thermal conductivity PEEK composites
| Serial number | Thermal conductivity (W/m ℃ C.) | Flexural modulus (GPa) | IZOD impact strength (kJ/square meter) | Heat distortion temperature (. degree. C.) |
| Example 1 | 0.89 | 22 | 8.52 | 380 |
| Example 2 | 0.86 | 23 | 8.45 | 380 |
| Example 3 | 0.86 | 22 | 8.92 | 379 |
| Example 4 | 0.88 | 24 | 9.05 | 382 |
| Example 5 | 0.90 | 24 | 9.85 | 383 |
| Example 6 | 0.87 | 25 | 10.3 | 385 |
Claims (6)
1. The high-thermal-conductivity polyether-ether-ketone composite material is characterized by comprising the following raw materials in parts by weight: 60-75 parts of polyether-ether-ketone, 5-10 parts of silicon carbide, 5-10 parts of boron nitride, 10-20 parts of basalt fiber and 0.5-1 part of antioxidant.
2. The composite material of claim 1, wherein the particle size of the polyetheretherketone, the silicon carbide and the boron nitride is 15-20 μm.
3. The composite material of claim 1, wherein the basalt fiber is a short fiber.
4. The high-thermal-conductivity polyetheretherketone composite material according to claim 3, wherein the basalt fiber is a short fiber of 8 to 10 mm.
5. The preparation method of the high-thermal-conductivity polyether-ether-ketone composite material is characterized by comprising the following steps of:
(1) and (3) drying: providing raw materials of the high-thermal-conductivity polyetheretherketone composite material according to claim 1, and respectively drying polyetheretherketone, silicon carbide, boron nitride and basalt fiber at the temperature of 180-190 ℃ for 5-6 h;
(2) mixing: uniformly mixing the dried polyether-ether-ketone, the silicon carbide, the boron nitride, the basalt fiber and the antioxidant;
(3) and (3) melt molding: and putting the mixed raw materials into a mold, pressurizing to 2-3 MPa, maintaining the pressure for 10-20 min, heating to 380-400 ℃, keeping the temperature and maintaining the pressure for 3-4 h, then decompressing, cooling to 80-90 ℃, demolding, heating the demolded molding material to 270-280 ℃, and keeping the temperature for 2-3 h to obtain the high-thermal-conductivity polyether-ether-ketone composite material.
6. The preparation method of the high thermal conductivity polyether ether ketone composite material according to claim 5, wherein a high-speed mixer is selected for mixing in the step (2), and the rotation speed of the high-speed mixer is controlled to be 900-1000 r/min for mixing for 20-30 min.
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| CN109880288B (en) * | 2019-03-21 | 2020-08-25 | 中国科学院兰州化学物理研究所 | Polyether-ether-ketone self-lubricating composite material and preparation method and application thereof |
| CN112934161A (en) * | 2021-01-28 | 2021-06-11 | 嘉兴京能科技有限责任公司 | Modified corrosion-resistant PEEK filler material for rectifying tower and production method and application thereof |
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