CN105219018A - A kind of preparation method of modified carbon fiber reinforced polyether ether ketone matrix material - Google Patents
A kind of preparation method of modified carbon fiber reinforced polyether ether ketone matrix material Download PDFInfo
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- CN105219018A CN105219018A CN201510657263.4A CN201510657263A CN105219018A CN 105219018 A CN105219018 A CN 105219018A CN 201510657263 A CN201510657263 A CN 201510657263A CN 105219018 A CN105219018 A CN 105219018A
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Abstract
The invention provides a kind of preparation method of modified carbon fiber reinforced polyether ether ketone matrix material, comprising: 1) infiltrated in the extracting solution of organic solvent by carbon fibre tow, must remove photoresist carbon fiber; The carbon fiber that will remove photoresist infiltrates in water/Ursol D mixed solution, adds Isopentyl nitrite, stirs, filtration and washing; 2) carbon nano-particles is dispersed in water by ultrasonic method, carbon fiber is infiltrated in the dispersion liquid of carbon nano-particles, adds Isopentyl nitrite, stir, filter cleaning; 3) by the mixing raw material of polyether-ether-ketone and processing aid and modified carbon fiber in twin screw extruder, through melt extruding, granulation, to obtain final product.The present invention adopts diazonium salt to react activated carbon fibre, and by carbon nano-particles load at carbon fiber surface, improves carbon fiber surface activity, improves the wetting property of fiber and interlaminar resin; Modified carbon fiber and PEEK interlaminar resin have good mechanical bonding force, can effectively improve the mechanical properties such as the stretching of matrix material.
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material.
Background technology
Polyether-ether-ketone (PEEK) resin is a kind of special engineering plastics of excellent performance, compared with other special engineering plastics, there is more significant advantages, resistance to positive high temperature 260 DEG C, mechanical property are excellent, self lubricity is good, chemicals-resistant burn into is fire-retardant, peel resistance, wear resistance, radioprotective etc., and superpower mechanical property makes it can be used for the fields such as high-end machinery, automobile, nuclear engineering and aviation.Therefore, polyether-ether-ketone (PEEK) resin is one of preferred high-end resin of field of compound material.
Carbon fiber is performance resins based composites reinforcement the most frequently used at present, has low density, the advantage such as high specific strength, high ratio modulus, high temperature resistant, resistance to chemical attack and thermal expansivity are little.Carbon-fibre composite is also widely used in the aspects such as aerospace, military affairs, machinery, high-performance sports equipment, and effect is attracted attention by common people.
Because carbon fiber surface is level and smooth, active function groups is few, table and can be low, present surface chemistry inertia, poor with resin matrix wetting property, make composite material interface bounding force more weak, seriously have impact on the performance of composites excellent properties; At present, the method for carbon fiber surface modification mainly comprises liquid phase oxidation, vapour phase oxidation process, plasma oxidation, grafting, high-energy ray irradiation method etc.These methods can cause certain destruction to the surface tissue of carbon fiber usually, cause fiber bodies intensity to have certain decline; The shortcomings such as simultaneously these methods also have production capacity little, can not continuous seepage, seriously polluted.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material is provided.
Object of the present invention is achieved through the following technical solutions:
The object of the present invention is to provide a kind of preparation method of modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material, comprising:
(1) surface active of carbon fiber
Using organic solvent as extracting solution, be under the condition of 75 DEG C-85 DEG C in temperature, infiltrated in extracting solution by carbon fibre tow, mechanical stirring and/or ultrasonic 2-8h, then filtering drying must remove photoresist carbon fiber;
The carbon fiber that will remove photoresist infiltrates in water/Ursol D mixed solution, mechanical stirring is also heated to 60 DEG C-90 DEG C, then under agitation, slowly adds Isopentyl nitrite, after completing, continuation stirs 12-24h under 60-90 DEG C of condition, and filtration and washing obtains the carbon fiber of aniline activation;
(2) carbon fiber surface load nano particle
Carbon nano-particles is dispersed in water by ultrasonic method, the carbon fiber activated by aniline infiltrates in the dispersion liquid of carbon nano-particles, be heated to 60-90 DEG C and stir condition under, slowly add Isopentyl nitrite, and 12-24h is stirred under the condition of 60-90 DEG C, filter and clean to obtain the carbon fiber of area load nanoparticle;
(3) preparation of modified carbon fiber reinforced polyether ether ketone
Raw material is chosen by following weight part:
Polyether-ether-ketone 55-85 part;
Modified carbon fiber 10-40 part;
Processing aid 1-5 part;
Polyether-ether-ketone is mixed with processing aid, obtains mixing raw material; Then join twin screw extruder from main spout, side spout respectively by mixing raw material and modified carbon fiber, through melt extruding, granulation, obtains described modified carbon fiber reinforced polyether ether ketone matrix material.
Extracting solution described in step (1) is selected from the mixing solutions of one or more in acetone, ethanol, sherwood oil, N ' dinethylformamide.
In water described in step (1)/Ursol D mixed solution, the massfraction of Ursol D is 1-3%; The mol ratio of Isopentyl nitrite and Ursol D is 1-3:3; The quality of carbon fiber of removing photoresist and the volume ratio of water/Ursol D mixed solution are 1-10g:500ml.
Carbon nano-particles described in step (2) is selected from the mixture of one or more in carbon nanotube, Graphene, graphene oxide, carbon nanofiber, and the carbon fiber of carbon nano-particles, aniline activation and the mass ratio of Isopentyl nitrite are 1-3:100:0.5-1.5; The concentration of the dispersion liquid of carbon nano-particles is 0.1-1g:500ml.
Processing aid described in step (3) is selected from one or more in fire retardant, toughner, conductive agent, antioxidant, photostabilizer, lubricant, tinting material, nucleator, static inhibitor, filler.
Twin screw extruder heating zone front-end temperature described in step (3) is 310-330 DEG C, and stage casing temperature is 340-370 DEG C, and terminal temperature is 330-360 DEG C, and rotating speed is 150-300rpm.
The preparation method of modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material that the present invention proposes activates carbon fiber surface, at carbon fiber surface grafting aniline molecule chain with diazonium salt reaction.Again under the effect of catalyzer, by the method for chemical graft by functional nanoparticle load at carbon fiber surface.Afterwards, twin screw extruder is adopted to carry out extruding pelletization to modified carbon fiber and polyether-ether-ketone (PEEK).Diazonium salt reaction, under the prerequisite affecting carbon fiber bulk strength not significantly, adds the surfactivity point of carbon fiber, and improves the wetting property of carbon fiber and PEEK resin.By surfactivity point as anchor point, by functional nanoparticle load at carbon fiber surface, the mechanical bond ability of fortifying fibre and resin, the final mechanical property such as stretching, impact, bending and interlayer shear effectively improving matrix material.
Compared with prior art, positively effect of the present invention is as follows:
1) adopt diazonium salt reaction activated carbon fibre, and by carbon nano-particles load at carbon fiber surface, improve carbon fiber surface activity, improve the wetting property of fiber and interlaminar resin, can't significantly reduce carbon fiber bulk strength;
2) modified carbon fiber and PEEK interlaminar resin have good mechanical bonding force, can effectively improve the mechanical properties such as the stretching of matrix material.
Accompanying drawing explanation
Fig. 1 is that carbon fiber SEM schemes, wherein, a () original carbon fiber, (b) remove photoresist carbon fiber, (c) aniline activated carbon fibre, (d) different concns aniline activated carbon fibre, (e) load graphene carbon fiber, (f) load carbon nanotube carbon fiber.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) surface active of carbon fiber
Using acetone as extracting solution, be heated to 80 DEG C, infiltrated in extracting solution by carbon fibre tow, ultrasonic 2h, and mechanical stirring 2h, filter afterwards and use a large amount of deionized water rinsing, and oven dry can be removed photoresist carbon fiber;
It is in the water/Ursol D mixed solution of 1.5% (Ursol D 0.69mol) that carbon fiber after being removed photoresist by 100g infiltrates at the massfraction of 5L, is heated to 80 DEG C, and mechanical stirring.Under agitation, 40g (0.345mol) Isopentyl nitrite is slowly added.After completing, continuation stirs 12h under 80 DEG C of conditions, filter and with a large amount of deionized water rinsing obtain aniline activation carbon fiber;
(2) carbon fiber surface load nano particle
1g Graphene is dispersed in 5L water by ultrasonic method, 100g aniline activated carbon fibre is infiltrated in the dispersion liquid of Graphene, be heated to 80 DEG C and stir condition under, slowly add the Isopentyl nitrite of 0.5g, and 12h is stirred under the condition of 80 DEG C, filter the carbon fiber that cleaning obtains area load Graphene.
(3) preparation of modified carbon fiber reinforced polyether ether ketone (PEEK)
Raw material is chosen by following weight part:
Polyether-ether-ketone (PEEK): 85 parts;
Modified carbon fiber: 10 parts;
Processing aid: 5 parts;
Polyether-ether-ketone (PEEK) is mixed with processing aid, obtains mixing raw material; Add in twin screw extruder through major ingredient mouth and pressure side spout respectively by mixing raw material and modified carbon fiber, through melt extruding, granulation, obtains modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material.
Processing aid comprises: fire retardant 1 part, antioxidant 1 part, lubricant 1 part, filler 2 parts.Forcing machine heating zone front-end temperature is 320 DEG C, and stage casing temperature is 360 DEG C, and terminal temperature is 340 DEG C, and rotating speed is 200rpm.
Embodiment 2
(1) surface active of carbon fiber
Using acetone/N ' dinethylformamide mixing solutions as extracting solution, be heated to 75 DEG C, infiltrated in extracting solution by carbon fibre tow, mechanical stirring 8h, filters afterwards and uses a large amount of deionized water rinsing, and oven dry can be removed photoresist carbon fiber;
It is in water/Ursol D (Ursol D 1.38mol) mixed solution of 3% that carbon fiber after being removed photoresist by 100g infiltrates at the massfraction of 5L, is heated to 90 DEG C, and mechanical stirring.Under agitation, 80g (0.69mol) Isopentyl nitrite is slowly added.After completing, continuation stirs 12h under 90 DEG C of conditions, filter and with a large amount of deionized water rinsing obtain aniline activation carbon fiber.
(2) carbon fiber surface load nano particle
1g multi-walled carbon nano-tubes is dispersed in 5L water by ultrasonic method, 100g aniline activated carbon fibre is infiltrated in the dispersion liquid of Graphene, be heated to 80 DEG C and stir condition under, slowly add the Isopentyl nitrite of 0.5g, and 12h is stirred under the condition of 80 DEG C, filter the carbon fiber that cleaning obtains area load carbon nanotube.
(3) preparation of modified carbon fiber reinforced polyether ether ketone (PEEK)
Raw material is chosen by following weight part:
Polyether-ether-ketone (PEEK): 70 parts;
Modified carbon fiber: 25 parts;
Processing aid: 5 parts;
Polyether-ether-ketone (PEEK) is mixed with processing aid, obtains mixing raw material; Add in twin screw extruder through major ingredient mouth and pressure side spout respectively by mixing raw material and modified carbon fiber, through melt extruding, granulation, obtains modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material.
Processing aid comprises: solid lubricant 2 parts, antioxidant 1 part, fire retardant 1 part, filler 1 part.Forcing machine heating zone front-end temperature is 330 DEG C, and stage casing temperature is 370 DEG C, and terminal temperature is 350 DEG C, and rotating speed is 250rpm.
Embodiment 3
(1) surface active of carbon fiber
Using acetone as extracting solution, be heated to 85 DEG C, infiltrated in extracting solution by carbon fibre tow, ultrasonic 2h, filters afterwards and uses a large amount of deionized water rinsing, and oven dry can be removed photoresist carbon fiber;
It is in the water/Ursol D mixed solution of 2.5% (Ursol D 1.16mol) that carbon fiber after being removed photoresist by 100g infiltrates at the massfraction of 5L, is heated to 70 DEG C, and mechanical stirring.Under agitation, 67.7g (0.58mol) Isopentyl nitrite is slowly added.After completing, continuation stirs 12h under 70 DEG C of conditions, filter and with a large amount of deionized water rinsing obtain aniline activation carbon fiber;
(2) carbon fiber surface load nano particle
1g graphene oxide is dispersed in 5L water by ultrasonic method, 100g aniline activated carbon fibre is infiltrated in the dispersion liquid of Graphene, be heated to 75 DEG C and stir condition under, slowly add the Isopentyl nitrite of 0.5g, and 12h is stirred under the condition of 75 DEG C, filter the carbon fiber that cleaning obtains area load Graphene.
(3) preparation of modified carbon fiber reinforced polyether ether ketone (PEEK)
Raw material is chosen by following weight part:
Polyether-ether-ketone (PEEK): 60 parts;
Modified carbon fiber: 35 parts;
Processing aid: 5 parts;
Polyether-ether-ketone (PEEK) is mixed with processing aid, obtains mixing raw material; Add in twin screw extruder through major ingredient mouth and pressure side spout respectively by mixing raw material and modified carbon fiber, through melt extruding, granulation, obtains modified carbon fiber reinforced polyether ether ketone (PEEK) matrix material.
Processing aid comprises: fire retardant 1 part, antioxidant 1.5 parts, lubricant 1.5 parts, filler 1 part.Forcing machine heating zone front-end temperature is 310 DEG C, and stage casing temperature is 340 DEG C, and terminal temperature is 360 DEG C, and rotating speed is 300rpm.
The actual measurement mechanical property parameters of embodiment 1-3 is in table 1.
Table 1
Claims (6)
1. a preparation method for modified carbon fiber reinforced polyether ether ketone matrix material, comprising:
(1) surface active of carbon fiber
Using organic solvent as extracting solution, be under the condition of 75 DEG C-85 DEG C in temperature, infiltrated in extracting solution by carbon fibre tow, mechanical stirring and/or ultrasonic 2-8h, then filtering drying must remove photoresist carbon fiber;
The carbon fiber that will remove photoresist infiltrates in water/Ursol D mixed solution, mechanical stirring is also heated to 60 DEG C-90 DEG C, then under agitation, adds Isopentyl nitrite, after completing, continuation stirs 12-24h under 60-90 DEG C of condition, and filtration and washing obtains the carbon fiber of aniline activation;
(2) carbon fiber surface load nano particle
Carbon nano-particles is dispersed in water by ultrasonic method, the carbon fiber activated by aniline infiltrates in the dispersion liquid of carbon nano-particles, be heated to 60-90 DEG C and stir condition under, add Isopentyl nitrite, and 12-24h is stirred under the condition of 60-90 DEG C, filter and clean to obtain the carbon fiber of area load nanoparticle;
(3) preparation of modified carbon fiber reinforced polyether ether ketone
Raw material is chosen by following weight part:
Polyether-ether-ketone 55-85 part;
Modified carbon fiber 10-40 part;
Processing aid 1-5 part;
Polyether-ether-ketone is mixed with processing aid, obtains mixing raw material; Then join twin screw extruder from main spout, side spout respectively by mixing raw material and modified carbon fiber, through melt extruding, granulation, obtains described modified carbon fiber reinforced polyether ether ketone matrix material.
2. the preparation method of a kind of modified carbon fiber reinforced polyether ether ketone matrix material according to claim 1, is characterized in that: the extracting solution described in step (1) is selected from the mixing solutions of one or more in acetone, ethanol, sherwood oil, N ' dinethylformamide.
3. the preparation method of a kind of modified carbon fiber reinforced polyether ether ketone matrix material according to claim 1, is characterized in that: in the water described in step (1)/Ursol D mixed solution, the massfraction of Ursol D is 1-3%; The mol ratio of Isopentyl nitrite and Ursol D is 1-3:3; The quality of carbon fiber of removing photoresist and the volume ratio of water/Ursol D mixed solution are 1-10g:500ml.
4. the preparation method of a kind of modified carbon fiber reinforced polyether ether ketone matrix material according to claim 1, it is characterized in that: the carbon nano-particles described in step (2) is selected from the mixture of one or more in carbon nanotube, Graphene, graphene oxide, carbon nanofiber, the carbon fiber of carbon nano-particles, aniline activation and the mass ratio of Isopentyl nitrite are 1-3:100:0.5-1.5; The concentration of the dispersion liquid of carbon nano-particles is 0.1-1g:500ml.
5. the preparation method of a kind of modified carbon fiber reinforced polyether ether ketone matrix material according to claim 1, is characterized in that: the processing aid described in step (3) is selected from one or more in fire retardant, toughner, conductive agent, antioxidant, photostabilizer, lubricant, tinting material, nucleator, static inhibitor, filler.
6. the preparation method of a kind of modified carbon fiber reinforced polyether ether ketone matrix material according to claim 1, it is characterized in that: the twin screw extruder heating zone front-end temperature described in step (3) is 310-330 DEG C, stage casing temperature is 340-370 DEG C, terminal temperature is 330-360 DEG C, and rotating speed is 150-300rpm.
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| CN106751443A (en) * | 2016-11-23 | 2017-05-31 | 大连路阳科技开发有限公司 | The corrosion-resistant friction-resistant composite material of metallic plastic-lining and preparation method and application |
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| CN108102292A (en) * | 2017-12-05 | 2018-06-01 | 宜宾天原集团股份有限公司 | A kind of preparation method of conduction polyether-ether-ketone composite material |
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| CN108102292A (en) * | 2017-12-05 | 2018-06-01 | 宜宾天原集团股份有限公司 | A kind of preparation method of conduction polyether-ether-ketone composite material |
| CN108744050A (en) * | 2018-06-29 | 2018-11-06 | 中南大学 | A method of improving polyether-ether-ketone and polyvinyl alcohol Composite Bone mount interface binding performance using graphene oxide |
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| CN111533931A (en) * | 2020-05-18 | 2020-08-14 | 东华大学 | CF/PEEK composite material with full transverse crystal structure and preparation method thereof |
| CN111533931B (en) * | 2020-05-18 | 2021-03-26 | 东华大学 | CF/PEEK composite material with full transverse crystal structure and preparation method thereof |
| CN112457629A (en) * | 2020-11-30 | 2021-03-09 | 吉林大学 | Carbon fiber surface grafted two-dimensional network structure reinforced polyether-ether-ketone composite material and preparation method thereof |
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Application publication date: 20160106 |