CN109627679A - A kind of highly conductive polyether-ether-ketone composite material and preparation method thereof - Google Patents
A kind of highly conductive polyether-ether-ketone composite material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of highly conductive polyether-ether-ketone composite material and preparation method thereof, belongs to macromolecule conducting material field.Highly conductive polyether-ether-ketone composite material provided by the invention, is made of the raw material of following parts by weight: 80-100 parts of PEEK, 10-20 parts of reinforcing fiber, 10-15 parts of grafted modified carbon nano tube, 3-8 parts of anti-wear agent, 2-5 parts of coupling agent, 0.5-1 parts of antioxidant, 1-2 parts of lubricant.The present invention is using PEEK as base-material, reinforcing fiber is added, carbon nanotube, anti-wear agent etc., the composite material of preparation not only has excellent mechanical property, high temperature resistant and wear-resisting property, while by carrying out grafting modification to carbon nanotube, assign composite material high conduction performance and high temperature appearance color stability.
Description
Technical field
The present invention relates to macromolecule conducting material field more particularly to a kind of highly conductive polyether-ether-ketone composite materials, can
Meet the highly conductive requirement of material.
Background technique
Conducting polymer composite material is by mixing conductive filler preparation in the polymer to insulation.Conductive filler includes
Metal and carbon system two major classes, the geometry state and conduction property of filler itself influence introduction, carbon system to the electrical property of composite material
Filler because of light weight, the advantages such as electrical property, Good Heat-resistance and intensity height and be widely used.Carbon nanotube
(CNTs) be carbon system filler a new classification, have high draw ratio, biggish specific surface area, excellent mechanical performance and
Unique photoelectric property, the composite material prepared by carbon nanotube and non-conductive polymer, can be excellent by carbon nanotube
The machined performance of mechanics and electrical property and polymer combines, and is with a wide range of applications.
Polyether-ether-ketone, abbreviation PEEK are the repetitive unit institute structures in backbone structure containing a ketonic bond and two ehter bonds
At high polymer, belong to new special engineering plastics, PEEK has high temperature resistant, and chemical resistance corrosion, not only heat resistance is than it
Its high-temperature resistance plastice is excellent, and has high intensity, high-modulus, high-fracture toughness and excellent dimensional stability, and
PEEK resin has tribological property outstanding, and resistance to skimming wear and Fretting are excellent, and PEEK also has self-lubrication
The excellent properties such as good, easy processing, insulating properties stabilization, hydrolysis, so that it is in aerospace, automobile manufacture, electric, medical
It is had a wide range of applications with fields such as food processings, exploitation prospect is very wide.
In addition the preparation of associate conductive composite material, such as prior art are also disclosed in the prior art
CN201510880586.X discloses a kind of polyphenylene sulfide/polyether-ether-ketone conducing composite material, including as follows by weight percent
The component of meter: polyphenylene sulfide/polyether-ether ketone polyblend 80-90%, polyphenylene sulfide/carbon material masterbatch 10-20%, by first by one
The carbon material carbon nanotube and graphene and polyphenylene sulfide for determining partial size are mixed with masterbatch, then mixs with matrix polymer, improvement
The dispersion and distribution of conductive filler in a polymer matrix.
Prior art CN201010611646.5 discloses a kind of highly conductive polymer carbon nanotube composites, including poly-
Object 50-99.95 parts of conjunction, 0.05-20 parts of carbon nanotube, 0-15 parts of antioxidant, 0-15 parts of dispersing agent, during micro machining
High temperature gradient field and shear rate gradient fields present in miniature molten chamber make polymer and carbon nanotube by friction, cut
It the processes such as cuts, spread and obtaining the good polymer of dispersion stabilization and carbon nano tube compound material.
The highly conductive polyether-ether-ketone composite material disclosed in the prior art is by first preparing masterbatch or passing through selection
Specific processing technology improves the dispersion performance of basis material and carbon nanotube, though to a certain extent can through the above way
The dispersion of carbon nanotube in the base is enough solved, but in practical application work, non-conductive polymer/carbon nanotube composite
There is also many obstacles, such as dispersion, interface problem and the stability of carbon nanotube in the base all not to obtain very for material
It is good to solve, and electric conductivity declines caused by can not solving in applied at elevated temperature because of the reunion of carbon nanotube, Yi Jiyan
The problem of colored appearance, to limit its scope of application.
Summary of the invention
The purpose of the present invention is provide in view of the deficiencies of the prior art a kind of highly conductive polyether-ether-ketone composite material and its
Processing method, the composite material not only have excellent mechanical property, high temperature resistant and wear-resisting property, while by carbon nanometer
Pipe carries out chemical modification, assigns composite material high conduction performance and high temperature appearance color stability.
In one embodiment of the invention, a kind of highly conductive polyether-ether-ketone composite material is provided, by following parts by weight
The group of number is grouped as:
80-100 parts of PEEK
10-20 parts of reinforcing fiber
10-15 parts of grafted modified carbon nano tube
3-8 parts of anti-wear agent
2-5 parts of coupling agent
0.5-1 parts of antioxidant
1-2 parts of lubricant.
Wherein, the molecular weight Mw of the PEEK resin is between 50-100 ten thousand, and melt index is in 5-25g/10min；Choosing
The molecular weight and melt index for selecting PEEK resin are advantageous the mechanical property and processing performance that guarantee material.
The reinforcing fiber is one or both of carbon fiber, aramid fiber, and the addition of reinforcing fiber is for improving
Mechanical property, wear-resisting property and the high temperature resistance of material are advantageous.
The carbon nanotube partial size is the single-walled carbon nanotube or multi-walled carbon nanotube of 10-40nm, the addition of carbon nanotube
It can not only assign material excellent electric conductivity, while can also assign material excellent mechanical property.
The modified carbon nano-tube the preparation method is as follows:
(1) surface coupling agent of carbon nanotube is modified
A, coupling agent KH570 is added into the ethanol water that mass fraction is 50%, adjusting pH with dilute acid solution is
3-4 is configured to the KH570 coupling agent solution that mass fraction is 30%；
B, it is silane coupled that 10-20 parts of carbon nanotubes, 100-150 parts of acetone, 10-20 parts of KH570 are added into reaction vessel
Agent solution stirs evenly, and is stirred to react at 60-70 DEG C 5-8 hours；
C, it after reaction, filters, is washed with anhydrous propanone, it is dry, obtain silane coupler modified carbon nanotube；
(2) modified carbon nano-tube surface graft modification
D, 10-15 parts of modified carbon nano-tubes, 50-120 parts of methyl methacrylates, 20-30 parts of benzene are added into reactor
Ethylene, 200-300 parts of acetone, stirring, and it is warming up to 70-80 DEG C；
E, 0.5-1.0 parts of initiators, stirring heat preservation 1-3 hours is added；
F, 100 DEG C are warming up at insulation reaction 4-8 hours；
G, with drying after acetone washing product, the carbon nanotube of surface graft modification is obtained.
The initiator is one of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate.
Silane coupling agent KH570 is first passed through in the present invention to be modified carbon nano tube surface, then passes through silane coupling agent
On double bond and methyl methacrylate, graft polymerization, change the polarity of system, and methyl methacrylate-benzene
Ethylene copolymer also has good comprehensive mechanical property, which is introduced into carbon nanotube, can significantly improve and gathers
The interface interaction of ether ether ketone is conducive to improve composite material to facilitate the loading and stably dispersing of increase carbon nanotube
Electric conductivity, mechanical property and high temperature appearance stablity performance.
The anti-wear agent is nanometer silicon carbide, nano magnesia, nano silica, nano boron carbide, nano oxidized
One or more of aluminium, further preferably through coupling agent modified anti-wear agent；The anti-wear agent of selection has high rigidity, low mill
Characteristics such as damage, while also there is preferable thermal conduction characteristic, can frictional heat caused by Decentralized Friction material in time, polymerization can be reduced
The thermal degradation of object improves the service life of composite material.
The coupling agent is selected from one or more of silane coupling agent, titanate coupling agent.
The lubricant is one or more of polytetrafluoroethylene (PTFE), molybdenum disulfide, graphite, silicone, wherein poly- four
Vinyl fluoride and silicone belong to organic polymer lubricant, have good lubricating action, can reduce adhesive wear；Curing
Molybdenum, graphite are then preferable solid lubricants, have the function of stablizing coefficient of friction, while can reduce the abrasion of material.
In another embodiment of the present invention, a kind of preparation side of highly conductive polyether-ether-ketone composite material is additionally provided
Method, specifically includes the following steps:
(1) PEEK is dried at 150-160 DEG C, dry 2-3 hours spare；
(2) by dried PEEK, reinforcing fiber, grafted modified carbon nano tube, anti-wear agent, coupling agent, antioxidant, lubrication
Agent is added high-speed mixer and is mixed, and obtains mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
Therefore, the present invention provides a kind of highly conductive polyether-ether-ketone composite material, has the advantage that
Highly conductive polyether-ether-ketone composite material component provided by the invention contains the carbon nanotube of surface graft modification, gram
It has taken carbon nanotube and has dispersed irregular, dispersion defect that is unstable and reducing composite materials property and electric conductivity, simultaneously
Merging for carbon nanotube and polymeric matrix material is also promoted, while being also avoided that by the mixed and modified carbon nanotube of simple physical
Caused by high temperature reunite occur stain, thus the problem of influencing the appearance of material.
Specific embodiment
It is that the purpose of the present invention, technical solution and advantage is more clearly understood convenient for the further explanation present invention, with
Under in conjunction with specific embodiments, the present invention is further described in detail.It should be appreciated that specific implementation described herein
Example does not limit the present invention only to explain the present invention.
Use the molecular weight of PEEK for 600,000 in the present invention in embodiment and comparative example, melt flow rate (MFR) 20g/
10min；The partial size of carbon nanotube is 20nm.
Embodiment 1
The present embodiment provides a kind of highly conductive polyether-ether-ketone composite materials, are grouped as by the group of following parts by weight number:
80 parts of PEEK, 10 parts of aramid fiber, 10 parts of grafted modified carbon nano tube, 5 parts of nano aluminium oxide, silane coupling agent 2
Part, 0.5 part of antioxidant, 1 part of polytetrafluoroethylene (PTFE).
Wherein grafted modified carbon nano tube is prepared via a method which:
A, coupling agent KH570 is added into the ethanol water that mass fraction is 50%, adjusting pH with dilute acid solution is
3.5, it is configured to the KH570 coupling agent solution that mass fraction is 30%；
B, 15 parts of carbon nanotubes, 120 parts of acetone, 15 parts of KH570 silane coupler solutions, stirring are added into reaction vessel
Uniformly, and at 60 DEG C it is stirred to react 6 hours；
C, it after reaction, filters, is washed with anhydrous propanone, it is dry, obtain silane coupler modified carbon nanotube；
(2) modified carbon nano-tube surface graft modification
D, addition 10 parts of modified carbon nano-tubes, 70 parts of methyl methacrylates, 20 parts of styrene into reactor, 200 parts
Acetone, stirring, and it is warming up to 70 DEG C；
E, 0.8 part of initiator, stirring heat preservation 2 hours is added；
F, 100 DEG C are warming up at insulation reaction 5 hours；
G, with drying after acetone washing product, the carbon nanotube of surface graft modification is obtained.
The highly conductive polyether-ether-ketone composite material the preparation method is as follows:
(1) PEEK of formula ratio is taken to be dried at 150 DEG C, dry 2 hours spare；
(2) according to formulation dosage by dried PEEK, aramid fiber, grafted modified carbon nano tube, nano aluminium oxide, silicon
Alkane coupling agent, antioxidant, polytetrafluoroethylene (PTFE) are added high-speed mixer and are mixed, and obtain mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
Embodiment 2
The present embodiment provides a kind of highly conductive polyether-ether-ketone composite materials, are grouped as by the group of following parts by weight number:
100 parts of PEEK, 18 parts of carbon fiber, 15 parts of grafted modified carbon nano tube, 6 parts of nanometer silicon carbide, silane coupling agent 4
Part, 1 part of antioxidant, 0.5 part of molybdenum disulfide, 0.5 part of graphite.
Wherein grafted modified carbon nano tube is prepared via a method which:
A, coupling agent KH570 is added into the ethanol water that mass fraction is 50%, adjusting pH with dilute acid solution is
3.5, it is configured to the KH570 coupling agent solution that mass fraction is 30%；
B, 20 parts of carbon nanotubes, 150 parts of acetone, 20 parts of KH570 silane coupler solutions, stirring are added into reaction vessel
Uniformly, and at 70 DEG C it is stirred to react 5 hours；
C, it after reaction, filters, is washed with anhydrous propanone, it is dry, obtain silane coupler modified carbon nanotube；
(2) modified carbon nano-tube surface graft modification
D, addition 15 parts of modified carbon nano-tubes, 100 parts of methyl methacrylates, 30 parts of styrene into reactor, 300 parts
Acetone, stirring, and it is warming up to 80 DEG C；
E, 1 part of initiator, stirring heat preservation 2 hours is added；
F, 100 DEG C are warming up at insulation reaction 6 hours；
G, with drying after acetone washing product, the carbon nanotube of surface graft modification is obtained.
The highly conductive polyether-ether-ketone composite material the preparation method is as follows:
(1) PEEK of formula ratio is taken to be dried at 150 DEG C, dry 2 hours spare；
(2) according to formulation dosage by dried PEEK, carbon fiber, grafted modified carbon nano tube, nanometer silicon carbide, silane
Coupling agent, antioxidant, molybdenum disulfide and graphite are added high-speed mixer and are mixed, and obtain mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
Comparative example 1
The present embodiment provides a kind of highly conductive polyether-ether-ketone composite materials, are grouped as by the group of following parts by weight number:
80 parts of PEEK, 10 parts of aramid fiber, 10 parts of modified carbon nano-tube, 5 parts of nano aluminium oxide, 2 parts of silane coupling agent,
0.5 part of antioxidant, 1 part of polytetrafluoroethylene (PTFE).
Wherein modified carbon nano-tube is prepared via a method which:
A, coupling agent KH570 is added into the ethanol water that mass fraction is 50%, adjusting pH with dilute acid solution is
3.5, it is configured to the KH570 coupling agent solution that mass fraction is 30%；
B, 15 parts of carbon nanotubes, 120 parts of acetone, 15 parts of KH570 silane coupler solutions, stirring are added into reaction vessel
Uniformly, and at 60 DEG C it is stirred to react 6 hours；
C, it after reaction, filters, is washed with anhydrous propanone, it is dry, obtain silane coupler modified carbon nanotube；
The highly conductive polyether-ether-ketone composite material the preparation method is as follows:
(1) PEEK of formula ratio is taken to be dried at 150 DEG C, dry 2 hours spare；
(2) according to formulation dosage that dried PEEK, aramid fiber, modified carbon nano-tube, nano aluminium oxide, silane is even
Connection agent, antioxidant, polytetrafluoroethylene (PTFE) are added high-speed mixer and are mixed, and obtain mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
Comparative example 2
The present embodiment provides a kind of highly conductive polyether-ether-ketone composite materials, are grouped as by the group of following parts by weight number:
100 parts of PEEK, 18 parts of carbon fiber, 15 parts of grafted modified carbon nano tube, 6 parts of nanometer silicon carbide, silane coupling agent 4
Part, 1 part of antioxidant, 0.5 part of molybdenum disulfide, 0.5 part of graphite.
Wherein grafted modified carbon nano tube is prepared via a method which:
The preparation of grafted modified carbon nano tube
A, addition 15 parts of carbon nanotubes, 100 parts of methyl methacrylates, 30 parts of styrene into reactor, 300 part third
Ketone, stirring, and it is warming up to 80 DEG C；
B, 1 part of initiator, stirring heat preservation 2 hours is added；
C, 100 DEG C are warming up at insulation reaction 6 hours；
D, with drying after acetone washing product, the carbon nanotube of surface graft modification is obtained.
The highly conductive polyether-ether-ketone composite material the preparation method is as follows:
(1) PEEK of formula ratio is taken to be dried at 150 DEG C, dry 2 hours spare；
(2) according to formulation dosage by dried PEEK, carbon fiber, grafted modified carbon nano tube, nanometer silicon carbide, silane
Coupling agent, antioxidant, molybdenum disulfide and graphite are added high-speed mixer and are mixed, and obtain mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
Performance detection:
Performance inspection is carried out to highly conductive polyether-ether-ketone composite material obtained in embodiment 1-2 and comparative example 1-2 respectively
It surveys, testing result is as shown in table 1, and wherein properties examination criteria is respectively as follows:
Volume resistivity: using EST121 type number ultra-high resistance, micro current instrument, surveys according to GB/T1410-2006
Examination；
High temperature colour stability, using following evaluation criterion:
By obtained material product at 200 DEG C, roasts 24 hours, visually observe product surface stain quantity, and carry out
Classification is compared, and evaluation criterion is as follows:
Stain quantity 10 or less 1 grade
Stain quantity 10-50 or black color spot 5 or less 2 grades that diameter 1-5mm occur
Stain quantity 50 or more or occur black color spot 5-10 3 grades of diameter 1-5mm
Stain quantity is intensive or a large amount of diameter 1-5mm black colour tables occurs or the black color spot 4 of diameter 5mm or more occurs
Grade.
Table 1 implements the composition and performance test results of 1-2 and comparative example 1-2 composite material
From the result in table 1 it is found that by using the method for the present invention preparation graft modification carbon nanotube addition, gram
It has taken carbon nanotube and has dispersed that irregular, dispersion is unstable and reduces lacking for conductivity of composite material energy and high temperature colour stability
It falls into, volume resistivity of the invention reaches 4.2 × 102Ω cm shows good electric conductivity, while showing excellent
High temperature Color Stability.
Above embodiment is merely exemplary to illustrate the principle of the present invention and its effect, and is not intended to limit the present invention.It is all
The equivalent transformation done using present specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (10)
1. a kind of highly conductive polyether-ether-ketone composite material is grouped as by the group of following parts by weight number:
80-100 parts of PEEK
10-20 parts of reinforcing fiber
10-15 parts of grafted modified carbon nano tube
3-8 parts of anti-wear agent
2-5 parts of coupling agent
0.5-1 parts of antioxidant
1-2 parts of lubricant.
2. highly conductive polyether-ether-ketone composite material according to claim 1, which is characterized in that the graft modification carbon is received
Mitron is prepared with the following method:
(1) surface coupling agent of carbon nanotube is modified
A, coupling agent KH570 is added into the ethanol water that mass fraction is 50%, adjusting pH with dilute acid solution is 3-4,
It is configured to the KH570 coupling agent solution that mass fraction is 30%；
B, it is molten that 10-20 parts of carbon nanotubes, 100-150 parts of acetone, 10-20 parts of KH570 silane coupling agents are added into reaction vessel
Liquid stirs evenly, and is stirred to react at 60-70 DEG C 5-8 hours；
C, it after reaction, filters, is washed with anhydrous propanone, it is dry, obtain silane coupler modified carbon nanotube；
(2) modified carbon nano-tube surface graft modification
D, 10-15 parts of modified carbon nano-tubes, 50-120 parts of methyl methacrylates, 20-30 parts of styrene are added into reactor,
200-300 parts of acetone, stirring, and it is warming up to 70-80 DEG C；
E, 0.5-1.0 parts of initiators, stirring heat preservation 1-3 hours is added；
F, 100 DEG C are warming up at insulation reaction 4-8 hours；
G, with drying after acetone washing product, the carbon nanotube of surface graft modification is obtained.
3. highly conductive polyether-ether-ketone composite material according to claim 2, which is characterized in that the initiator is over cure
One of sour ammonium, potassium peroxydisulfate, sodium peroxydisulfate.
4. highly conductive polyether-ether-ketone composite material according to claim 2, which is characterized in that the carbon nanotube is grain
Diameter is the single wall or multi-walled carbon nanotube of 10-40nm.
5. highly conductive polyether-ether-ketone composite material according to claim 1-4, which is characterized in that the PEEK
The molecular weight Mw of resin is between 50-100 ten thousand, and melt index is in 5-25g/10min.
6. highly conductive polyether-ether-ketone composite material according to claim 1-5, which is characterized in that the enhancing is fine
Dimension is one or both of carbon fiber, aramid fiber.
7. highly conductive polyether-ether-ketone composite material according to claim 1-6, which is characterized in that described is wear-resisting
Agent is one or more of nanometer silicon carbide, nano magnesia, nano silica, nano boron carbide, nano aluminium oxide.
8. highly conductive polyether-ether-ketone composite material according to claim 1-7, which is characterized in that
The coupling agent is selected from one or more of silane coupling agent, titanate coupling agent.
9. highly conductive polyether-ether-ketone composite material according to claim 1-8, which is characterized in that
The lubricant is one or more of polytetrafluoroethylene (PTFE), molybdenum disulfide, graphite, silicone.
10. the preparation method of the described in any item highly conductive polyether-ether-ketone composite materials of preceding claims 1-9, feature exist
In, comprising the following steps:
(1) PEEK is dried at 150-160 DEG C, dry 2-3 hours spare；
(2) dried PEEK, reinforcing fiber, grafted modified carbon nano tube, anti-wear agent, coupling agent, antioxidant, lubricant are added
Enter high-speed mixer to be mixed, obtains mixture；
(3) highly conductive polyether-ether-ketone composite material is prepared by injection molding in the mixture that step (2) obtains.
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| CN201811328142.5A CN109627679A (en) | 2018-11-09 | 2018-11-09 | A kind of highly conductive polyether-ether-ketone composite material and preparation method thereof |
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| CN110339402A (en) * | 2019-07-29 | 2019-10-18 | 武汉理工大学 | The polyether-ether-ketone Biocomposite material and preparation method thereof of α phase nano aluminium oxide enhancing |
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| CN110595302B (en) * | 2019-09-19 | 2021-11-02 | 西安庆华民用***器材股份有限公司 | Preparation method of delay element for detonator |
| CN110591283A (en) * | 2019-09-30 | 2019-12-20 | 新奥（内蒙古）石墨烯材料有限公司 | Conductive graphene composite material and preparation method and application thereof |
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| CN112829344A (en) * | 2020-12-31 | 2021-05-25 | 江苏亨博复合材料有限公司 | PEEK material based on carbon fiber reinforced type and preparation equipment thereof |
| CN112812497A (en) * | 2020-12-31 | 2021-05-18 | 江苏亨博复合材料有限公司 | Wear-resistant PEEK composite material |
| CN115304902A (en) * | 2021-04-07 | 2022-11-08 | 伊顿智能动力有限公司 | High toughness electrically conductive PEEK for aircraft fuel systems |
| CN113652057A (en) * | 2021-09-28 | 2021-11-16 | 吉林大学 | 3D printing high-strength high-toughness polyether-ether-ketone carbon nanotube composite material and preparation method thereof |
| CN113652057B (en) * | 2021-09-28 | 2022-06-21 | 吉林大学 | 3D printing high-strength high-toughness polyether-ether-ketone carbon nanotube composite material and preparation method thereof |
| CN113956560A (en) * | 2021-10-28 | 2022-01-21 | 王智辉 | High-strength heat-resistant polyethylene material and preparation method thereof |
| CN113956560B (en) * | 2021-10-28 | 2023-04-18 | 胜利油田兴达高祥新材料有限责任公司 | High-strength heat-resistant polyethylene material and preparation method thereof |
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| CN115975368A (en) * | 2022-12-08 | 2023-04-18 | 烯湾科城(广州)新材料有限公司 | MPPO composite material and preparation method thereof |
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