CN110527247B - Double-network polyether-ether-ketone composite material and preparation method and application thereof - Google Patents
Double-network polyether-ether-ketone composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of special engineering plastics, in particular to a double-network polyether-ether-ketone composite material and a preparation method and application thereof. The double-network polyether-ether-ketone composite material provided by the invention comprises a polyether-ether-ketone/multi-wall carbon nanotube composite material and graphene nanosheets; the polyether-ether-ketone/multi-walled carbon nanotube composite material is formed by dispersing multi-walled carbon nanotubes in polyether-ether-ketone; the polyether-ether-ketone/multi-walled carbon nanotube composite material is distributed in a network structure formed by the graphene nanosheets. According to the description of the embodiment, the double-network polyether-ether-ketone composite material has good thermal conductivity.
Description
Technical Field
The invention relates to the technical field of special engineering plastics, in particular to a double-network polyether-ether-ketone composite material and a preparation method and application thereof.
Background
With the rapid development of industries, the requirements of various industries on the heat conducting performance of materials are higher and higher. However, the conventional general-purpose plastics are limited by their low heat resistance and cannot meet some harsh use environments, such as: aerospace, military and automotive special parts, etc. Once the temperature is too high and heat is accumulated, the material can be softened and even damaged and deformed, thereby causing great safety hazard. Polyether ether ketone (PEEK) serving as a high-performance special engineering plastic can be safely used at 250 ℃ for a long time, can be used at 300 ℃ for a short time, and can meet a plurality of severe use requirements.
However, polyetheretherketone has a low thermal conductivity (0.25W/m.K) similar to that of other polymer materials. In order to improve the heat conductivity of PEEK, it is currently the most common way to blend inorganic heat conductive fillers, such as carbon material, boron nitride, and alumina, into PEEK, and the resulting composite material can have an order of magnitude of thermal conductivity improvement.
At present, researchers mainly prepare the heat-conducting polyether-ether-ketone composite material in a direct blending mode. Chinese patent with publication No. CN106243620A prepares a high-strength heat-conducting polyetheretherketone composite material by blending copper powder, aluminum oxide, aluminum nitride and short carbon fibers into the polyetheretherketone composite material; chinese patent with publication number CN107674376A prepares an insulating and heat-conducting polyether-ether-ketone cable material, and modified hexapotassium carbonate whisker and inorganic nano-filler are added into PEEK/PES to improve the heat-conducting capacity of the polyether-ether-ketone composite material.
However, the composite materials obtained by the above preparation methods cannot ensure the dispersibility of the blend in polyetheretherketone, and finally lead to a limited improvement of the thermal conductivity.
Disclosure of Invention
The invention aims to provide a double-network polyether-ether-ketone composite material with better heat-conducting property.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a double-network polyether-ether-ketone composite material, which comprises a polyether-ether-ketone/multi-walled carbon nanotube composite material and graphene nanosheets;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is formed by dispersing multi-walled carbon nanotubes in polyether-ether-ketone;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is distributed in a network structure formed by the graphene nanosheets;
the network structure formed by the graphene nanosheets is a honeycomb-like structure.
Preferably, the mass ratio of the multi-wall carbon nanotubes to the polyetheretherketone/multi-wall carbon nanotube composite material in the polyetheretherketone/multi-wall carbon nanotube composite material is (0.1-6): 100.
preferably, the mass ratio of the polyether-ether-ketone/multi-walled carbon nanotube composite material to the graphene nanosheet is (80-99): (1-20).
The invention also provides a preparation method of the double-network polyether-ether-ketone composite material, which comprises the following steps:
mixing diphenyl sulfone, a multi-walled carbon nanotube, xylene, hydroquinone, 4' -difluorobenzophenone and a catalyst, and carrying out in-situ mixing construction to obtain a polyether-ether-ketone/multi-walled carbon nanotube composite material;
and mixing the polyether-ether-ketone/multi-walled carbon nanotube composite material with the graphene nanosheets, and performing ball milling and pressing in sequence to obtain the double-network polyether-ether-ketone composite material.
Preferably, the catalyst is one or more of sodium carbonate, potassium carbonate and cesium carbonate.
Preferably, the solid content of the raw material for in-situ mixing construction is 10-20%;
the molar ratio of hydroquinone to 4,4' -difluorobenzophenone to the catalyst is (0.9-1.1): (0.9-1.1): (0.9-1.2).
Preferably, the in-situ mixing construction process is as follows: the temperature is increased from room temperature to 300-310 ℃ in a gradient way;
the gradient temperature rise is divided into five stages, and the final temperatures of the five stages are 160-180 ℃, 210-230 ℃, 250-270 ℃, 280-300 ℃ and 300-310 ℃ respectively.
Preferably, the rotation speed of the ball mill is 300-400 rpm, and the time is 4-8 hours.
Preferably, the pressing temperature is 350-400 ℃, and the pressing pressure is 5-10 MPa.
The invention also provides the application of the double-network polyether-ether-ketone composite material in the technical scheme or the double-network polyether-ether-ketone composite material prepared by the preparation method in the technical scheme in the fields of electronics, automobile energy and aerospace.
The invention provides a double-network polyether-ether-ketone composite material, which comprises a polyether-ether-ketone/multi-walled carbon nanotube composite material and graphene nanosheets; the polyether-ether-ketone/multi-walled carbon nanotube composite material is formed by dispersing multi-walled carbon nanotubes in polyether-ether-ketone; the polyether-ether-ketone/multi-walled carbon nanotube composite material is distributed in a network structure formed by the graphene nanosheets. In the invention, the first network of the double-network polyether-ether-ketone composite material is a heat conduction network provided inside the polyether-ether-ketone/multi-walled carbon nanotube composite material, the second network is a honeycomb-like network formed by graphene nano sheets wrapped outside the polyether-ether-ketone/multi-walled carbon nanotube composite material, so that a compact heat conduction network is formed, meanwhile, the carbon nanotubes inside the network also form rich capillary heat conduction channels, and the heat transfer efficiency can be effectively increased through binary synergy and sodium micro-synergy, so that the heat conduction performance of the material is greatly improved. According to the description of the embodiment, the axial thermal conductivity coefficient of the double-network polyether-ether-ketone composite material is not less than 0.42W/(m.K), and the radial thermal conductivity coefficient is not less than 1.05W/(m.K).
Drawings
FIG. 1 is a flow chart of the preparation process of the double-network polyetheretherketone composite material of the present invention.
Detailed Description
The invention provides a double-network polyether-ether-ketone composite material, which comprises a polyether-ether-ketone/multi-walled carbon nanotube composite material and graphene nanosheets;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is formed by dispersing multi-walled carbon nanotubes in polyether-ether-ketone;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is distributed in a network structure formed by the graphene nanosheets;
the network structure formed by the graphene nanosheets is a honeycomb-like structure. (the concrete structure is as shown in FIG. 1 for the final product structure in the preparation process)
In the invention, the mass ratio of the multi-wall carbon nanotube to the polyetheretherketone/multi-wall carbon nanotube composite material in the polyetheretherketone/multi-wall carbon nanotube composite material is preferably (0.1-6): 100, more preferably (1-4): 100, most preferably (2-3): 100, respectively; the mass ratio of the polyether-ether-ketone/multi-walled carbon nanotube composite material to the graphene nanosheet is preferably (80-99): (1-20), more preferably (85-95): (5-15), most preferably (88-92): (8-12).
The invention also provides a preparation method of the double-network polyether-ether-ketone composite material, which comprises the following steps:
mixing diphenyl sulfone, a multi-walled carbon nanotube, xylene, hydroquinone, 4' -difluorobenzophenone and a catalyst, and carrying out in-situ mixing construction to obtain a polyether-ether-ketone/multi-walled carbon nanotube composite material;
and mixing the polyetheretherketone/multi-walled carbon nanotube composite material and the graphene nanosheets, and performing ball milling and pressing in sequence to obtain the double-network polyetheretherketone composite material (the specific preparation flow is shown in fig. 1).
In the invention, the catalyst is one or more of sodium carbonate, potassium carbonate and cesium carbonate, and when the catalyst is more than two of the above specific choices, the proportion of the specific substances is not limited in any way. The preparation method comprises the steps of mixing diphenyl sulfone, multi-walled carbon nanotubes, xylene, hydroquinone, 4' -difluorobenzophenone and a catalyst, and carrying out in-situ mixing construction to obtain a polyether-ether-ketone/multi-walled carbon nanotube composite material; in the invention, the molar ratio of hydroquinone, 4' -difluorobenzophenone and the catalyst is preferably (0.9-1.1): (0.9-1.1): (0.9-1.2), more preferably 1:1: 1; the mass ratio of the xylene to the diphenyl sulfone is preferably (20-50): 100, more preferably (25-45): 100, most preferably (30-40): 100. in the present invention, the solid content of the raw material system for the in-situ mixing construction is preferably 10% to 20%, more preferably 12% to 18%, and most preferably 14% to 16%.
In the invention, the mixing process is preferably to mix the multi-walled carbon nanotube and xylene for 1-2 hours under the ultrasonic condition, and then mix the obtained mixture with diphenyl sulfone, hydroquinone, 4' -difluorobenzophenone and a catalyst; the present invention does not have any particular limitation on the frequency of the ultrasound, and an ultrasound frequency known to those skilled in the art may be used. In the present invention, the mixing is preferably carried out in a three-necked flask. In the present invention, the in-situ mixing construction is preferably performed under an argon atmosphere; the in-situ mixing construction process is preferably as follows: the temperature is increased from room temperature to 300-310 ℃ in a gradient way; the gradient temperature rise is preferably divided into five stages, and the final temperatures of the five stages are 160-180 ℃, 210-230 ℃, 250-270 ℃, 280-300 ℃ and 300-310 ℃ respectively. In the invention, the degassing treatment is preferably carried out before the temperature is increased to 160-180 ℃, and the degassing treatment is preferably carried out by mechanically stirring for 0.5-1.5 hours. After the temperature is increased to 160-180 ℃, preferably preserving the heat for 2-4 hours, and continuously increasing the temperature to 210-230 ℃; the invention has no special limitation on the heat preservation time within the temperature range of 210-230 ℃, and the xylene in the reaction system can be removed completely by adopting the time well known by the technical personnel in the field; and after the xylene is completely removed, continuously heating to 250-270 ℃, keeping the temperature for 1-2 hours, then continuously heating to 280-300 ℃, keeping the temperature for 1-2 hours, and finally heating to 300-310 ℃ until the viscosity of the reaction system is unchanged. The temperature rise rate in each stage is not particularly limited in the present invention, and a temperature rise rate known to those skilled in the art may be used.
After the in-situ mixing construction is completed, the obtained product system is preferably subjected to post-treatment, and the post-treatment is preferably performed by mixing the product system with deionized water to precipitate the polyetheretherketone/multi-walled carbon nanotube composite material, and then sequentially drying, crushing, washing and ball-milling. The present invention is not limited to any particular drying, pulverization, and washing. In the invention, the time for ball milling is preferably 4-8 hours, and more preferably 5-6 hours; the purpose of ball milling is to enable the particle size of the obtained polyetheretherketone/multi-walled carbon nanotube composite material to be within the range of 100-200 microns.
After the polyether-ether-ketone/multi-walled carbon nanotube composite material is obtained, the polyether-ether-ketone/multi-walled carbon nanotube composite material and the graphene nanosheets are mixed, and ball milling and pressing are sequentially performed to obtain the double-network polyether-ether-ketone composite material. The mixing is not particularly limited in the present invention, and may be carried out by a mixing process known to those skilled in the art. In the invention, the rotation speed of the ball milling is preferably 300-400 rpm, more preferably 320-380 rpm, and most preferably 340-360 rpm, the time of the ball milling is preferably 4-8 hours, more preferably 5-6 hours, the ball-to-material ratio of the ball milling is preferably 1:1, and the diameter of the steel ball used for the ball milling is 5 mm.
After the ball milling is completed, the invention preferably removes the part with the size larger than 100 microns and smaller than 500 microns by using a sieve with the aperture of 100 microns and 500 microns.
In the invention, the pressing temperature is preferably 350-450 ℃, more preferably 380-420 ℃, and most preferably 400 ℃, and the pressing pressure is preferably 5-10 MPa, more preferably 6-8 MPa.
The pressing process is preferably as follows: heating to the pressing temperature, keeping the temperature for 10min, pressurizing to the pressing pressure, keeping the pressure for 10min, and slowly cooling to room temperature; the temperature rising rate and the temperature reducing rate of temperature rise and temperature reduction are not limited in any way, and the temperature rising rate and the temperature reducing rate which are well known to those skilled in the art can be adopted.
The invention also provides the application of the double-network polyether-ether-ketone composite material in the technical scheme or the double-network polyether-ether-ketone composite material prepared by the preparation method in the technical scheme in the fields of electronics, automobile energy and aerospace.
The following examples are provided to illustrate the bis-network polyetheretherketone composite material and the preparation method and application thereof, but they should not be construed as limiting the scope of the present invention.
Example 1
Under the condition of ultrasound, 2.23g of multi-walled carbon nanotube and 70g of xylene are mixed for 1 hour, the obtained mixture is mixed with 220mL of diphenyl sulfone, 27.53g of hydroquinone, 55.45g of 4,4' -difluorobenzophenone, 30.21g of sodium carbonate and 2.1g of potassium carbonate, the mixture is stirred for 0.5 hour under the protection of argon gas for degassing, the temperature is raised to 170 ℃, azeotropic dehydration reflux is carried out for 2 hours, the temperature is raised to 210 ℃, xylene is removed, the temperature is continuously raised to 250 ℃, the temperature is kept for 1 hour, the temperature is continuously raised to 280 ℃, the temperature is kept for 1 hour, the obtained product system is mixed with deionized water until the product system is not changed, the polyetheretherketone/multi-walled carbon nanotube composite material is separated out, drying, crushing and washing are carried out to obtain the polyetheretherketone/multi-walled carbon nanotube composite material, finally the polyetheretherketone/multi-walled carbon nanotube composite material is ground for 4 hours, obtaining a polyether-ether-ketone/multi-walled carbon nanotube composite material of 100-200 microns;
mixing 8g of a 100-200 micron polyetheretherketone/multiwall carbon nanotube composite material and 2g of graphene nanosheets, ball-milling (5mm steel balls, the ball-material ratio is 1:1, and the rotation speed is 375rpm) for 4 hours, then performing press forming (heating to 370 ℃, keeping the temperature for 10min, pressurizing for 5MPa, and keeping the pressure for 10min), and slowly cooling to room temperature to obtain a double-network polyetheretherketone composite material, which is marked as PEEK/3MWCNT 20 GNS.
Example 2
Under the condition of ultrasound, 3g of multi-walled carbon nanotube and 70g of xylene are mixed for 1 hour, the obtained mixture is mixed with 220mL of diphenyl sulfone, 27.53g of hydroquinone, 55.45g of 4,4' difluorobenzophenone, 30.21g of sodium carbonate and 2.1g of potassium carbonate, the mixture is stirred for 0.5 hour under the protection of argon gas for degassing, the temperature is raised to 170 ℃, azeotropic dehydration reflux is carried out for 2 hours, the temperature is raised to 210 ℃, after the xylene is removed, the temperature is continuously raised to 250 ℃, the temperature is kept for 1 hour, the temperature is continuously raised to 280 ℃, the temperature is finally raised to 310 ℃, the temperature is kept until the product system is unchanged, the obtained product system is mixed with deionized water to precipitate the polyetheretherketone/multi-walled carbon nanotube composite material, then the drying, crushing and washing are carried out to obtain the polyetheretherketone/multi-walled carbon nanotube composite material, and finally the polyetheretherketone/multi-walled carbon nanotube composite material is ground for, obtaining a polyether-ether-ketone/multi-walled carbon nanotube composite material of 100-200 microns;
mixing 8g of a 100-200 micron polyetheretherketone/multiwall carbon nanotube composite material and 2g of graphene nanosheets, ball-milling (5mm steel balls, the ball-material ratio is 1:1, and the rotation speed is 375rpm) for 4 hours, then performing compression molding (heating to 370 ℃, keeping the temperature for 10min, pressurizing for 5MPa, and keeping the pressure for 10min), and slowly cooling to room temperature to obtain a double-network polyetheretherketone composite material, which is marked as PEEK/4MWCNT @ CNT 20 GNS.
Example 3
Under the condition of ultrasound, 3g of multi-walled carbon nanotube and 70g of xylene are mixed for 1 hour, the obtained mixture is mixed with 220mL of diphenyl sulfone, 27.53g of hydroquinone, 55.45g of 4,4' difluorobenzophenone, 30.21g of sodium carbonate and 2.1g of potassium carbonate, the mixture is stirred for 0.5 hour under the protection of argon gas for degassing, the temperature is raised to 170 ℃, azeotropic dehydration reflux is carried out for 2 hours, the temperature is raised to 210 ℃, after the xylene is removed, the temperature is continuously raised to 250 ℃, the temperature is kept for 1 hour, the temperature is continuously raised to 280 ℃, the temperature is finally raised to 310 ℃, the temperature is kept until the product system is unchanged, the obtained product system is mixed with deionized water to precipitate the polyetheretherketone/multi-walled carbon nanotube composite material, then the drying, crushing and washing are carried out to obtain the polyetheretherketone/multi-walled carbon nanotube composite material, and finally the polyetheretherketone/multi-walled carbon nanotube composite material is ground for, obtaining a polyether-ether-ketone/multi-walled carbon nanotube composite material of 100-200 microns;
mixing 8.5g of a 100-200 micron polyetheretherketone/multiwall carbon nanotube composite material and 1.5g of graphene nanosheets, ball-milling (5mm steel ball, ball-material ratio of 1:1, rotation speed of 375rpm) for 4 hours, press-forming (heating to 370 ℃, keeping the temperature for 10min, pressurizing to 5MPa, keeping the pressure for 10min), and slowly cooling to room temperature to obtain a double-network polyetheretherketone composite material, which is recorded as PEEK/4MWCNT @15 GNS.
Example 4
Under the condition of ultrasound, 3g of multi-walled carbon nanotube and 70g of xylene are mixed for 1 hour, the obtained mixture is mixed with 220mL of diphenyl sulfone, 27.53g of hydroquinone, 55.45g of 4,4' difluorobenzophenone, 30.21g of sodium carbonate and 2.1g of potassium carbonate, the mixture is stirred for 0.5 hour under the protection of argon gas for degassing, the temperature is raised to 170 ℃, azeotropic dehydration reflux is carried out for 2 hours, the temperature is raised to 210 ℃, after the xylene is removed, the temperature is continuously raised to 250 ℃, the temperature is kept for 1 hour, the temperature is continuously raised to 280 ℃, the temperature is finally raised to 310 ℃, the temperature is kept until the product system is unchanged, the obtained product system is mixed with deionized water to precipitate the polyetheretherketone/multi-walled carbon nanotube composite material, then the drying, crushing and washing are carried out to obtain the polyetheretherketone/multi-walled carbon nanotube composite material, and finally the polyetheretherketone/multi-walled carbon nanotube composite material is ground for, obtaining a polyether-ether-ketone/multi-walled carbon nanotube composite material of 100-200 microns;
mixing 9.0g of a 100-200 micron polyetheretherketone/multiwall carbon nanotube composite material with 1.0g of graphene nanosheets, ball-milling (5mm steel ball, ball-material ratio of 1:1, rotation speed of 375rpm) for 4 hours, press-forming (heating to 370 ℃, keeping the temperature for 10min, pressurizing for 5MPa, keeping the pressure for 10min), and slowly cooling to room temperature to obtain a double-network polyetheretherketone composite material, which is recorded as PEEK/4MWCNT @10 GNS.
Example 5
Under the condition of ultrasound, 3g of multi-walled carbon nanotube and 70g of xylene are mixed for 1 hour, the obtained mixture is mixed with 220mL of diphenyl sulfone, 27.53g of hydroquinone, 55.45g of 4,4' difluorobenzophenone, 30.21g of sodium carbonate and 2.1g of potassium carbonate, the mixture is stirred for 0.5 hour under the protection of argon gas for degassing, the temperature is raised to 170 ℃, azeotropic dehydration reflux is carried out for 2 hours, the temperature is raised to 210 ℃, after the xylene is removed, the temperature is continuously raised to 250 ℃, the temperature is kept for 1 hour, the temperature is continuously raised to 280 ℃, the temperature is finally raised to 310 ℃, the temperature is kept until the product system is unchanged, the obtained product system is mixed with deionized water to precipitate the polyetheretherketone/multi-walled carbon nanotube composite material, then the drying, crushing and washing are carried out to obtain the polyetheretherketone/multi-walled carbon nanotube composite material, and finally the polyetheretherketone/multi-walled carbon nanotube composite material is ground for, obtaining a polyether-ether-ketone/multi-walled carbon nanotube composite material of 100-200 microns;
mixing 9.5g of a 100-200 micron polyetheretherketone/multiwall carbon nanotube composite material with 0.5g of graphene nanosheets, ball-milling (5mm steel ball, ball-material ratio of 1:1, rotation speed of 375rpm) for 4 hours, press-forming (heating to 370 ℃, keeping the temperature for 10min, pressurizing to 5MPa, keeping the pressure for 10min), and slowly cooling to room temperature to obtain a double-network polyetheretherketone composite material, which is recorded as PEEK/4MWCNT @5 GNS.
Comparative example 1
Mixing 0.08g of multi-walled carbon nanotube, 7.92g of polyether-ether-ketone and 2g of graphene nanosheet, performing ball milling for 4 hours, performing compression molding (heating to 370 ℃, keeping the temperature for 10min, then pressurizing for 5MPa, and keeping the pressure for 10min), and slowly cooling to room temperature to obtain the polyether-ether-ketone composite material.
Test example
According to the GBT-22588 standard, the thermal conductivity of the dual-network polyetheretherketone composite materials obtained in examples 1-5 and comparative example 1 was tested, and the test results are shown in tables 1-2:
TABLE 1 thermal conductivity of the dual network polyetheretherketone composites obtained in examples 1 to 5 and comparative example 1
According to the embodiments, the double-network polyether-ether-ketone composite material provided by the invention has good thermal conductivity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A double-network polyether-ether-ketone composite material is characterized by comprising a polyether-ether-ketone/multi-wall carbon nanotube composite material and graphene nanosheets;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is formed by dispersing multi-walled carbon nanotubes in polyether-ether-ketone;
the polyether-ether-ketone/multi-walled carbon nanotube composite material is distributed in a network structure formed by the graphene nanosheets;
the network structure formed by the graphene nanosheets is a honeycomb-like structure;
the preparation method of the double-network polyether-ether-ketone composite material comprises the following steps:
mixing diphenyl sulfone, a multi-walled carbon nanotube, xylene, hydroquinone, 4' -difluorobenzophenone and a catalyst, and carrying out in-situ mixing construction to obtain a polyether-ether-ketone/multi-walled carbon nanotube composite material;
and mixing the polyether-ether-ketone/multi-walled carbon nanotube composite material with the graphene nanosheets, and performing ball milling and pressing in sequence to obtain the double-network polyether-ether-ketone composite material.
2. The dual-network polyetheretherketone composite material of claim 1, wherein the weight ratio of the multi-wall carbon nanotubes to the polyetheretherketone/multi-wall carbon nanotube composite material is (0.1-6): 100.
3. the double-network polyetheretherketone composite material of claim 1 or 2, wherein the polyetheretherketone/multiwall carbon nanotube composite material and graphene nanoplatelets are present in a mass ratio of (80-99): (1-20).
4. The preparation method of the double-network polyether-ether-ketone composite material as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
mixing diphenyl sulfone, a multi-walled carbon nanotube, xylene, hydroquinone, 4' -difluorobenzophenone and a catalyst, and carrying out in-situ mixing construction to obtain a polyether-ether-ketone/multi-walled carbon nanotube composite material;
and mixing the polyether-ether-ketone/multi-walled carbon nanotube composite material with the graphene nanosheets, and performing ball milling and pressing in sequence to obtain the double-network polyether-ether-ketone composite material.
5. The method of claim 4, wherein the catalyst is one or more of sodium carbonate, potassium carbonate and cesium carbonate.
6. The method of claim 4, wherein the raw material for the in-situ mixing is 10-20% solid;
the molar ratio of hydroquinone to 4,4' -difluorobenzophenone to the catalyst is (0.9-1.1): (0.9-1.1): (0.9-1.2).
7. The method of claim 4, wherein the in-situ mixing is performed by: the temperature is increased from room temperature to 300-310 ℃ in a gradient way;
the gradient temperature rise is divided into five stages, and the final temperatures of the five stages are 160-180 ℃, 210-230 ℃, 250-270 ℃, 280-300 ℃ and 300-310 ℃ respectively.
8. The method of claim 4, wherein the ball milling is performed at a speed of 300 to 400rpm for 4 to 8 hours.
9. The method according to claim 4, wherein the pressing temperature is 350 to 400 ℃ and the pressing pressure is 5 to 10 MPa.
10. Use of the bis-network polyetheretherketone composite material according to any of claims 1 to 3 or prepared by the preparation method according to any of claims 4 to 9 in the fields of electronics, automotive energy and aerospace.
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