CN106565887A - Carbon fiber reinforced thermoplastic resin composite material and preparation method thereof - Google Patents
Carbon fiber reinforced thermoplastic resin composite material and preparation method thereof Download PDFInfo
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- CN106565887A CN106565887A CN201510638621.7A CN201510638621A CN106565887A CN 106565887 A CN106565887 A CN 106565887A CN 201510638621 A CN201510638621 A CN 201510638621A CN 106565887 A CN106565887 A CN 106565887A
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Abstract
The invention provides a carbon fiber reinforced thermoplastic resin composite material and a preparation method thereof. The carbon fiber reinforced thermoplastic resin composite material provided by the invention comprises a polystyrene copolymer and continuous carbon fiber. The preparation method provided by the invention comprises steps of impregnation and in-situ polymerization, wherein the step of impregnation is to impregnate the continuous carbon fiber in a resin composition which comprises 5 to 30 wt% of the polystyrene copolymer and 95 to 70 wt% of a styrene monomer and a copolymerization monomer; and the step of in-situ polymerization is to polymerize the above-mentioned impregnated system at 60 to 180 DEG C for 2 to 20 h. The fiber reinforced thermoplastic resin composite material provided by the invention has the advantages of uniform material structure and low manufacturing cost. The preparation method provided by the invention has the advantages of low manufacturing cost, applicability to large-scale production, uniform structure of the obtained composite material, no use of a solvent, and good thermoplastic molding.
Description
Technical field
The present invention relates to the preparation method of fibre reinforced thermoplas tic resin composite and the fibre reinforced thermoplas tic resin composite obtained by the method.
Background technology
Since the seventies in last century, with the continuous improvement of carbon fiber performance, resin-based carbon fiber composite（carbon fiber reinforced
plastics, CFRP）Through lasting in-depth study and exploitation, most important aerospace structural material is nowadays had become, obtained a wide range of applications in field of aerospace.Due to the characteristic of its high-strength light, carbon fibre composite its usage amount in new airline carriers of passengers Boeing 787 and Air Passenger A380 has been up to 35 tons/frame, and the ratio for accounting for aircraft construction material has been over 50%.But on the other hand, with high costs due to its, up to the present in addition to a small amount of sports equipment for top grade, its application is also essentially confined to aerospace field to carbon fibre composite.
In recent years; it is increasingly serious with energy problem and environmental problem; people urgently expect that the carbon fibre composite of high-strength light can on a large scale be applied to the fields such as transportation, wind-power electricity generation, power-equipment; wish the reduction of discharging that lowers consumption by the lightweight of material, alleviating energy crisis and control environmental pollution.But current carbon fibre composite（CFRP）The overwhelming majority is carbon fiber-reinforced thermosetting resin composite materials（carbon fiber reinforced
Thermosetting composites, CFRTS）, in the extensive expanded application to other field following four big bottlenecks are faced：（1）The machine-shaping cycle is long, and working (machining) efficiency is low；（2）High cost：The high cost of thermosetting resin base carbon fiber composite material is not just merely because its raw material --- the high price of carbon fiber, but more from the high of its manufacturing cost；（3）Poor toughness：Because the matrix resin of CFRTS is thermosetting resin, therefore its impact property is poor；（4）Hardly possible is repaired, and hardly possible is reclaimed；It is insoluble after thermosetting resin base carbon fiber composite material is processed not melt, it is difficult to repair during damage；Still thermosetting resin is not recyclable when discarded, and the recycling of carbon fiber is also highly difficult.
In view of this, the government of countries in the world, enterprise and research institution all put into one after another huge fund and develop new resin system, innovation forming processing technology and equipment to break through these bottlenecks, seize the development first chance of this strategic industry of carbon fibre composite.Under this background, fibre reinforced thermoplas tic resin composite（carbon fiber reinforced
Thermoplastics, CFRTP）The visual field of people is progressed into.Need with thermosetting resin it is entirely different come curing molding by cross-linking reaction, thermoplastic resin only need to heat up melting soften, cooling hardened forming.The plasticizing forming process-cycle of thermoplastic resin typically in the several seconds to tens of seconds, than the curing molding cycle of thermosetting resin（Several minutes, even a few hours, a couple of days）Want much shorter.Thus, people expect that the moulding processability of CFRTP can have the raising of essence than CFRTS system, be more suitable for large-scale industrial production.
So far, the thermoplastic matrix resin for being combined with carbon fiber mainly has：PEEK（Polyether Ether Ketone）, PEKK（Polyether Ketone Ketone）, PPS（Polyphenylene Sulfide）, PEI（Polyether Imide）, PBT（Polybutylene Terephthalate）, PET（Polyethylene Terephthalate）, PC（Polycarbonate）, PAI（Polyamide Imide）, PP（Polypropylene）, TPI（Thermoplastic Polyimide）, N6（Nylon 6）And N66（Nylon 66）.General its molecular weight of thermoplastic resin is much higher compared with thermosetting resin prepolymer, and its mobility is more much lower than thermosetting resin prepolymer, thus it is to the immersion poorer than thermosetting resin prepolymer of carbon fiber.Its result is compound compound difficulty than thermosetting resin prepolymer to carbon fiber of the thermoplastic resin to carbon fiber, and compound tense is frequently necessary to some special measures in addition to high temperature and high pressure is needed, also.
The complex method of thermoplastic resin and carbon fiber mainly has：Solution impregnation, film laminating, fiber is mixed, and powder mixes and melt impregnation.Solution dipping method is exactly to select suitable solvent, by thermoplastic resin dissolving, is made into low viscous solution, the complex method for being impregnated to carbon fiber using the solution thereafter.Obviously, the method is suitable only for soluble thermoplastic's resin, and also requires that its solvent has suitable volatility, immersion condition it is not volatile and after the completion of dipping can far below resin oxidation, volatilize as soon as possible under decomposition temperature it is clean.Solution dipping method has the advantages that process is simple, low production cost, prepreg steady quality.Its shortcoming is then to use a large amount of solvents, can inevitably for operator and environment bring harm with removal process using；Furthermore, remove sweetening agent difficulty after the completion of dipping completely, and being retained in a small amount of solvent in prepreg can usually form bubble in composite molding, cause the surface defect and internal voids of material, consequently, it is possible to bringing hidden danger of quality to product.
Thin layer platen press is also a kind of complex method of the advanced composite material that is in daily use.By the way that carbon fiber is placed between the thin film of two layers of thermoplastic resin, the resin of melting is pressed between carbon fiber under uniform temperature and certain pressure, subsequently under stress cooling, consolidation complete to be combined.The advantage of the method is simple, reliable, environmental protection（Solvent is not used）.But, the method one is to need to ensure that prepreg has higher carbon fibrous body fraction using very thin thin film；Need very high pressure that resin could be pressed between fiber when being second laminated；Three lamination times will be grown and can be only achieved relatively low porosity.
Fiber mixing method is that first thermoplastic resin is spun into after fiber to mix with reinforcing fiber, forms composite fibre beam or hybrid yams.Its advantage is that the content of thermoplastic resin can be controlled accurately, and fiber is readily obtained fully infiltration, you can make prepreg tape to be molded, it is also possible to directly Wrapping formed to obtain product.But because some thermoplastic resins are difficult high cost for making diameter number μm fine fibre or producing fine fibre etc. and limit the application of this method.
Powder mixing process has two kinds of dry and wet, is after fiber is spread out, toner equably to be inhaled the surface for being attached to reinforcing fiber；Thereafter the carbon fiber of absorption powder is heated, pressurization and make thermoplastic resin by fibres bond, most after Jing consolidations, sizing and become prepreg.The damage of the method carbon fiber is less, it is also possible in extremely rapid succession prepare thermoplastic carbon fiber resin impregnated tape.But this law requires that resin must make powder, and requires that particle diameter is as little as possible（<10μm）, particle diameter it is as homogeneous as possible.
Melt impregnation is that thermoplastic resin heating is made into more low viscous melt, the method for subsequently carbon fiber for spreading out being carried out into impregnation process by the low viscosity thermoplastic resin melt.Melt impregnation is simple to operate, is widely used, and is a kind of very important dipping method.The method does not use solvent, thus can be avoided the high internal flaw of the void content caused due to the presence of solvent, is particularly well-suited to the preparation of the excellent thermoplastic resin prepreg tape of hot property.The requirement of melt impregnation mainly has two：（1）Melt viscosity of the thermoplastic resin used under dipping temperature is low, to there is higher surface tension, has preferable wellability with carbon fiber；（2）Thermoplastic resin answers holding structure to stablize under dipping temperature, does not aoxidize, does not decompose, does not react.The major defect of the method is that porosity is higher, and composite property is difficult to improve.
Melting pultrusion method refers to carbon fiber bundle by the tubulose melt tank that filled by thermoplastic melt, through the pultrusion of definite shape mouth mold into bar-shaped or lamellar prepreg.The method is grown up on the basis of melt impregnation, it is also possible to for the higher thermoplastic resin of melt viscosity.On the one hand can control gel content, reduce porosity using mouth mold, on the other hand it is also ensured that the uniformity of fiber distribution.But its working (machining) efficiency is low.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, there is provided a kind of fibre reinforced thermoplas tic resin composite, and material structure is uniform, and manufacturing cost is relatively low.
For achieving the above object, the technical scheme of fibre reinforced thermoplas tic resin composite employing of the present invention is：A kind of fibre reinforced thermoplas tic resin composite, it includes polystyrene copolymer and continuous carbon fibre.
It includes the continuous carbon fibre of polystyrene copolymer and volume content between 1%-60%.
The present invention is not particularly limited to the species of polystyrene copolymer, but the complexity of the performance and copolymerization in view of copolymer, the polystyrene copolymer is the mixture of one or more in styrene/acrylonitrile copolymer, phenylethylene ethylene/propenoic acid ester copolymer.
In view of the mechanical property of the too low then impact composite of molecular weight, the processing of too high then impact composite, the weight average molecular weight of the polystyrene copolymer is between 50,000-40 ten thousand.80,000-50 ten thousand can be further optimized for, optimum is 100,000-40 ten thousand.
In order to ensure the intensity of composite, the volume content of the continuous carbon fibre is 10-50%.Preferably, the volume content of the continuous carbon fibre is 20-50%.
Continuous carbon fibre is carbon fiber bundle, carbon fiber felt or carbon cloth.
The present invention also provides a kind of preparation method of fibre reinforced thermoplas tic resin composite, and low cost of manufacture is adapted to large-scale production, and the composite structure of acquisition is uniform, does not adopt solvent, and thermoplastic molding is good.
A kind of preparation method of fibre reinforced thermoplas tic resin composite, comprises the steps：（1）Impregnation：Continuous carbon fibre is immersed in resin combination, impregnation system is obtained, the volume content of continuous carbon fibre is 1%-60%；Wherein resin combination includes the polystyrene copolymer of 1-50wt%, and remaining is the mixture of styrene and comonomer；Comonomer can be acrylic acid, acrylic acid methyl ester., ethyl acrylate, butyl acrylate, 1-Octyl acrylate, acrylonitrile, methacrylic acid, methyl methacrylate, ethyl methacrylate, butyl methacrylate, one or more in 2-Propenoic acid, 2-methyl-, octyl ester；Preferably acrylic acid, acrylic acid methyl ester., ethyl acrylate, butyl acrylate, acrylonitrile, methacrylic acid, methyl methacrylate, ethyl methacrylate, one or more in butyl methacrylate；
（2）In-situ polymerization：By step（1）The impregnation system for obtaining temperature zone heating from low to high in 50-230 DEG C, polymerization time adds up to 2-30h.
Impregnation refers to and continuous carbon fibre is immersed in resin combination；The resinous polymer is the compositionss of polystyrene copolymer, styrene monomer and comonomer, it is contemplated that impact of the viscosity of resin combination to impregnation performance, further optimization, and the content of polystyrene copolymer is 5-35wt% in resin combination.
Optimization, the content of polystyrene copolymer is 10-30wt% in resin combination.
Viscosity at 25 DEG C of the resin combination is 50-50000mPa*s.
For the impregnation for having reached, the viscosity at 25 DEG C of resin combination is 100-50000mPa*s.
Further optimization, the viscosity at 25 DEG C of resin combination is 500-50000mPa*s.
In-situ polymerization refers to that styrene and comonomer in the composite that will be impregnated with carry out combined polymerization so as to be converted into polymer as far as possible, the temperature range of in-situ polymerization is 60-200 DEG C；In view of efficiency, polymerization time in view of styrene and the conversion ratio and molecular weight of copolymer of comonomer, can further be optimized, temperature range 60-180 DEG C with more short better, and polymerization time is 2-20h.
The present invention compared with prior art, with advantages below：
The preparation method of fibre reinforced thermoplas tic resin composite of the present invention, preparation efficiency is high, does not adopt the working condition of high temperature, high pressure, reduces manufacture difficulty, convenient to carry out, is adapted to scale industrial production.Do not adopt in solvent, therefore the fibre reinforced thermoplas tic resin composite for obtaining and do not contain solvent, the good product quality and steady quality after molding, the composite conjugation obtained by copolyreaction is high, and uniform in material, the strength of materials is high.
Specific embodiment
With reference to specific embodiment, further elucidate the present invention, it should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention, after the present invention has been read, modification of the those skilled in the art to the various equivalent form of values of the present invention falls within the application claims limited range.
In below example, materials described below has been used as raw material：
Styrene:99%, 4- containing 10-15ppm tert-butyl catechol stabilizer, purchased from Shanghai Aladdin biochemical technology limited company；
Acrylic acid methyl ester., ethyl acrylate, acrylic acid, purchased from Chinese medicines group；
Acrylonitrile, purchased from Chinese medicines group；
Carbon cloth：YT-3K-X200, purchased from Yixing City Yi Tai carbon fiber weavings company limited.
The preparation of resin combination
Embodiment 1：240ml acrylonitrile and 760ml styrene are added in 2l there-necked flasks under nitrogen protection, Jing after nitrogen displacement 3 times, under nitrogen atmosphere system are heated to into 80 DEG C, now polymerization starts.It is polymerized after reaching 5% to monomer conversion, system is dropped to rapidly room temperature, obtains thermoplastic resin composition A.
Embodiment 2：240ml methyl methacrylates and 760ml styrene are added in 2l there-necked flasks under nitrogen protection, Jing after nitrogen displacement 3 times, under nitrogen atmosphere system are heated to into 80 DEG C, now polymerization starts.It is polymerized after reaching 10% to monomer conversion, system is dropped to rapidly room temperature, obtains thermoplastic resin composition B.
Embodiment 3：240ml ethyl methacrylate and 760ml styrene are added in 2l there-necked flasks under nitrogen protection, Jing after nitrogen displacement 3 times, under nitrogen atmosphere system are heated to into 80 DEG C, now polymerization starts.It is polymerized after reaching 20% to monomer conversion, system is dropped to rapidly room temperature, obtains thermoplastic resin composition C.
Embodiment 4：150ml acrylic acid and 850ml styrene are added in 2l there-necked flasks under nitrogen protection, Jing after nitrogen displacement 3 times, under nitrogen atmosphere system are heated to into 80 DEG C, now polymerization starts.It is polymerized after reaching 35% to monomer conversion, system is dropped to rapidly room temperature, obtains thermoplastic resin composition D.
It is prepared by fibre reinforced thermoplas tic resin composite
Embodiment 5：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by the thermoplastic resin composition A primings by vacuum of 50ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, plus pressure is sequentially heated to 80 DEG C and is polymerized 5 hours, 90 DEG C to be polymerized 5 hours, 120 DEG C to be polymerized 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C be polymerized 5 hours, cooling obtains product.Product section can be seen that in composite layer without obvious hole by metallography microscope sem observation, resin to the wellability of fiber very well, parcel it is complete.After taking 10g product chloroform dissolution resins, drying is weighed and obtains 6.74 grams of carbon cloths, and the volume content that carbon fiber can be estimated from it is 55%.Determined by GPC, obtain resin weight average molecular weight for 5.5 ten thousand.
Embodiment 6：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by the thermoplastic resin composition B primings by vacuum of 60ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, plus pressure is sequentially heated to 80 DEG C and is polymerized 5 hours, 90 DEG C to be polymerized 5 hours, 120 DEG C to be polymerized 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C be polymerized 5 hours, cooling obtains product.Product section can be seen that in composite layer without obvious hole by metallography microscope sem observation, resin to the wellability of fiber very well, parcel it is complete.After taking 10g product chloroform dissolution resins, drying is weighed and obtains 5.61 grams of carbon cloths, and the volume content that carbon fiber can be estimated from it is 43%.Determined by GPC, obtain resin weight average molecular weight for 7.8 ten thousand.
Embodiment 7：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by the thermoplastic resin composition C primings by vacuum of 70ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, plus pressure is sequentially heated to 80 DEG C and is polymerized 5 hours, 90 DEG C to be polymerized 5 hours, 120 DEG C to be polymerized 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C be polymerized 5 hours, cooling obtains product.Product section can be seen that in composite layer without obvious hole by metallography microscope sem observation, resin to the wellability of fiber very well, parcel it is complete.After taking 10g product chloroform dissolution resins, drying is weighed and obtains 3.97 grams of carbon cloths, and the volume content that carbon fiber can be estimated from it is 28%.Determined by GPC, obtain resin weight average molecular weight for 18.9 ten thousand.
Embodiment 8：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by the thermoplastic resin composition D primings by vacuum of 80ml in mould, by carbon cloth thorough impregnation.Subsequently mould is put into into hot press, plus pressure is sequentially heated to 80 DEG C and is polymerized 10 hours, 90 DEG C to be polymerized 5 hours, 120 DEG C to be polymerized 5 hours, 180 DEG C be polymerized 5 hours, cooling obtains product.Product section can be seen that in composite layer without obvious hole by metallography microscope sem observation, resin to the wellability of fiber very well, parcel it is complete.After taking 10g product chloroform dissolution resins, drying is weighed and obtains 2.71 grams of carbon cloths, and the volume content that carbon fiber can be estimated from it is 18%.Determined by GPC, obtain resin weight average molecular weight for 35.6 ten thousand.
Claims (10)
1. a kind of fibre reinforced thermoplas tic resin composite, it is characterised in that it includes polystyrene copolymer and continuous carbon fibre.
2. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that:It includes the continuous carbon fibre of polystyrene copolymer and volume content between 1%-60%.
3. fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that:The polystyrene copolymer is the mixture of one or more in styrene/acrylonitrile copolymer, phenylethylene ethylene/propenoic acid ester copolymer.
4. fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that:The weight average molecular weight of the polystyrene copolymer is between 50,000-40 ten thousand.
5. fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that:The volume content of the continuous carbon fibre is 10-50%.
6. the preparation method of fibre reinforced thermoplas tic resin composite of claim 1-5 described in any one, it is characterised in that include following steps：
（1）Impregnation：Continuous carbon fibre is immersed in resin combination, impregnation system is obtained, the volume content of continuous carbon fibre is 1%-60%；Wherein resin combination includes the polystyrene copolymer of 1-50wt%, and remaining is the mixture of styrene and comonomer；
（2）In-situ polymerization：By step（1）The impregnation system for obtaining temperature zone heating from low to high in 50-230 DEG C, polymerization time adds up to 2-30h.
7. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：The content of polystyrene copolymer is 5-35wt% in resin combination.
8. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：The content of polystyrene copolymer is 10-30wt% in resin combination.
9. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：Viscosity at 25 DEG C of the resin combination is 50-50000mPa*s.
10. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：Viscosity at 25 DEG C of resin combination is 100-50000mPa*s.
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Application publication date: 20170419 |