CN106566099A - 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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- CN106566099A CN106566099A CN201510638659.4A CN201510638659A CN106566099A CN 106566099 A CN106566099 A CN 106566099A CN 201510638659 A CN201510638659 A CN 201510638659A CN 106566099 A CN106566099 A CN 106566099A
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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 includes polystyrene, unsaturated rubber and continuous carbon fibers. The preparation method comprises the following steps: 1, impregnating: impregnating the continuous carbon fibers in a resin composition to obtain an impregnation system, wherein the resin composition contains 0-30 wt% of polystyrene, 5-15 wt% of the unsaturated rubber and 95-55 wt% of a styrene monomer; and 2, carrying out in situ polymerization: polymerizing the impregnation system at 60-180 DEG C for 2-20 h. The fiber reinforced thermoplastic resin composite material has the advantages of uniform structure and low manufacturing cost. The preparation method has the advantages of low manufacturing cost, and suitableness for large-scale production, and the obtained composite material has a uniform structure, does not use a solvent, and has good thermoplastic formability.
Description
Technical field
The present invention relates to fibre reinforced thermoplas tic resin composite, further relates to the manufacture method of fibre reinforced thermoplas tic resin composite.
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, is 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 which, 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 be applied to the fields such as transportation, wind-power electricity generation, power-equipment on a large scale; wish by the lightweight of material come the reduction of discharging that lowers consumption, 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）, following four big bottlenecks are faced in the extensive expanded application to other field：（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：As the matrix resin of CFRTS is thermosetting resin, therefore its impact property is poor；（4）It is difficult to repair, it is difficult to reclaim；It is insoluble after thermosetting resin base carbon fiber composite material is processed not melt, it is difficult to repair during damage；When discarded, still thermosetting resin is not recyclable, 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 huge fund one after another 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 need to only 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 is mainly had：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 which is to the immersion poorer than thermosetting resin prepolymer of carbon fiber.The compound compound difficulty than thermosetting resin prepolymer to carbon fiber that its result is thermoplastic resin to carbon fiber, compound tense are 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 are 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 good solvent has suitable volatility, immersion condition it is not volatile and after the completion of dipping can far below resin oxidation, volatilize under decomposition temperature as soon as possible it is clean.Solution dipping method has the advantages that process is simple, low production cost, prepreg steady quality.Its shortcoming be then using a large amount of solvents, using and removal process in can inevitably for operator and environment bring harm；Furthermore, remove sweetening agent difficulty after the completion of dipping completely, and be retained in a small amount of solvent in prepreg and bubble can be usually formed in composite molding, cause the surface defect and internal voids of material, consequently, it is possible to hidden danger of quality is brought to product.
Thin layer platen press is also a kind of complex method of the advanced composite material that is in daily use.By 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 cooling, consolidation complete to be combined under stress.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 accurately can be controlled, 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 the application of this method is limited as some thermoplastic resins are difficult high cost made diameter number μm fine fibre or produce fine fibre etc..
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 more low viscous melt, the method that the carbon fiber for spreading out is carried out impregnation process by the low viscosity thermoplastic resin melt subsequently.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, will have higher surface tension, has preferable wellability with carbon fiber；（2）Under dipping temperature, thermoplastic resin answers holding structure stable, 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 gel content can be controlled, porosity is reduced 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, which includes polystyrene, unsaturated rubber and continuous carbon fibre.
Which includes the continuous carbon fibre of polystyrene, unsaturated rubber and volume content between 1%-60%.Unsaturated rubber is introduced in fibre reinforced thermoplas tic resin composite for improving the shock resistance of composite.
The too low mechanical property for then affecting composite of molecular weight, the too high processing for then affecting composite, the weight average molecular weight of polystyrene is 30,000-50 ten thousand.Preferably, the weight average molecular weight of polystyrene is 80,000-50 ten thousand, optimum is 100,000-40 ten thousand.
Described unsaturated rubber is one or more mixture in natural rubber, butadiene rubber, butyl rubber, butadiene-styrene rubber, nitrile rubber and neoprene.In view of the compatibility with polystyrene, unsaturated rubber is one or more mixture in butadiene rubber, butadiene-styrene rubber and neoprene.At least one most preferably in butadiene rubber, butadiene-styrene rubber.
Content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 1wt%-30wt%.Content of the unsaturated rubber in polystyrene and unsaturated rubber total amount（Content of the unsaturated rubber in resin base, that is, unsaturated rubber weight and polystyrene and the ratio of unsaturated rubber gross weight）, preferably, content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 3wt%-25wt%.
Content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 5wt%-15wt%.In order to ensure that rubber plays the effect for improving shock resistance, the content of rubber can not be too low, the rigidity on the other hand ensured by composite, then the content of rubber again can not be too high.
Used as further preferred, content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 5wt%-10wt%.
The volume content of the continuous carbon fibre is 10-50%.Preferably, the volume content of continuous carbon fibre is 20-50%.
The continuous carbon fibre is carbon fiber bundle, carbon fiber felt or carbon cloth.
Present invention also offers a kind of preparation method of fibre reinforced thermoplas tic resin composite, low cost of manufacture, are adapted to large-scale production, the composite structure of acquisition is uniform, does not contain solvent, and thermoplastic molding is good.
A kind of manufacture method of described fibre reinforced thermoplas tic resin composite, comprises the steps
（1）Impregnation：The continuous carbon fibre of the content is immersed in resin combination, impregnation system is obtained；Polystyrene containing 0-50wt% wherein in resin combination, the unsaturated rubber of 1-30wt%, remaining is styrene monomer；
（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 add up to 2-30h.
Content 0-30wt% of polystyrene, unsaturated rubber content 5wt%-15wt% in resin combination, remaining is styrene monomer.
Impregnation refers to and continuous carbon fibre is immersed in resin combination；Compositionss of the resinous polymer for polystyrene, styrene monomer and unsaturated rubber, in view of resin combination viscosity to be impregnated with performance impact, content 5-30wt% of polystyrene, unsaturated rubber content 5wt%-15wt% in described resin combination, remaining is styrene monomer.
Viscosity at 25 DEG C of the resin combination is 50-50000mPa*s.
For the impregnation for having reached, the viscosity that 25 degrees Celsius of resin combination is 100-50000mPa*s.
Preferably, the viscosity of 25 degrees Celsius of resin combination is 500-50000mPa*s.
In-situ polymerization refers to that the styrene monomer in the composite that will be impregnated with is polymerized so as to be converted into polymer as far as possible.In-situ polymerization temperature range 60-200 DEG C；In view of efficiency, polymerization time with more short better, while in view of the conversion ratio and molecular weight of styrene monomer, by step（1）Impregnation system at temperature range 60-180 DEG C stage feeding polymerization 2-20h.
The present invention compared with prior art, with advantages below：
Fibre reinforced thermoplas tic resin composite of the present invention does not adopt solvent, therefore solvent is not contained in the fibre reinforced thermoplas tic resin composite for obtaining, good product quality and steady quality after molding, the composite conjugation obtained by copolyreaction is high, uniform in material, the strength of materials is high, participates in reacting using unsaturated rubber, improves the shock resistance of fibre reinforced thermoplas tic resin composite.The preparation method of the present invention, preparation efficiency are high, do not adopt the working condition of high temperature, high pressure, reduce manufacture difficulty, convenient to carry out, are adapted to scale industrial production.
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 and comparative example, materials described below has been used as raw material：
Styrene monomer:99%, 4- containing 10-15ppm tert-butyl catechol stabilizer, purchased from Shanghai Aladdin biochemical technology limited company；
Butyl rubber, purchased from Yanshan Petrochemical；
Butadiene-styrene rubber, purchased from Ba Ling petrochemical industry；
Butadiene rubber, purchased from Gaoqiao Petrochemical Company；
Carbon cloth, purchased from YT-3K-X200, the Yixing City preferably limited public company of Thailand's carbon fiber weaving.
It is prepared by thermoplastic resin composition
Embodiment 1：Butadiene rubber after 150 grams are vacuum dried is put in 2l there-necked flasks, adds 939ml（850 grams）Styrene, under agitation by butadiene rubber swelling or dissolving；Thermoplastic resin composition A.
Embodiment 2：Butadiene-styrene rubber after 50 grams are vacuum dried is put in 2l there-necked flasks, adds 1049ml（950 grams）Styrene, under agitation by butadiene-styrene rubber swelling or dissolving；Jing after nitrogen displacement 3 times, system is heated to into 80 DEG C under nitrogen atmosphere, now polymerization starts.Be polymerized after 10% being reached to styrene conversion rate, system is dropped to rapidly room temperature, thermoplastic resin composition B is obtained.
Embodiment 3：Butyl rubber after 50 grams are vacuum dried is put in 2l there-necked flasks, adds 1049ml（950 grams）Styrene, under agitation by butyl rubber swelling or dissolving；Jing after nitrogen displacement 3 times, system is heated to into 80 DEG C under nitrogen atmosphere, now polymerization starts.Be polymerized after 20% being reached to styrene conversion rate, system is dropped to rapidly room temperature, thermoplastic resin composition C is obtained.
Embodiment 4：Butyl rubber after 50 grams are vacuum dried is put in 2l there-necked flasks, adds 1049ml（950 grams）Styrene, under agitation by butyl rubber swelling or dissolving；Jing after nitrogen displacement 3 times, system is heated to into 80 DEG C under nitrogen atmosphere, now polymerization starts.Be polymerized after 35% being reached to styrene conversion rate, system is dropped to rapidly room temperature, thermoplastic resin composition D is obtained.
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 thermoplastic resin composition's A primings by vacuum of 50ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 80 DEG C of polymerizations 5 hours, 90 DEG C of polymerizations is sequentially heated under pressurization and is polymerized within 5 hours, 120 DEG C 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C and is polymerized 5 hours, cooled down and obtain product.Product section is 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 6.38 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 51%.Determined by GPC, resin weight average molecular weight is obtained for 6.5 ten thousand.
Embodiment 6：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by thermoplastic resin composition's B primings by vacuum of 60ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 80 DEG C of polymerizations 5 hours, 90 DEG C of polymerizations is sequentially heated under pressurization and is polymerized within 5 hours, 120 DEG C 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C and is polymerized 5 hours, cooled down and obtain product.Product section is 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 5.51 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 42%.Determined by GPC, resin weight average molecular weight is obtained for 10.1 ten thousand.
Embodiment 7：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by thermoplastic resin composition's C primings by vacuum of 70ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 80 DEG C of polymerizations 5 hours, 90 DEG C of polymerizations is sequentially heated under pressurization and is polymerized within 5 hours, 120 DEG C 2.5 hours, 140 DEG C to be polymerized 2.5 hours, 180 DEG C and is polymerized 5 hours, cooled down and obtain product.Product section is 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 4.55 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 33%.Determined by GPC, resin weight average molecular weight is obtained for 15.3 ten thousand.
Embodiment 8：The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by thermoplastic resin composition's D primings by vacuum of 80ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 80 DEG C of polymerizations 10 hours, 90 DEG C of polymerizations is sequentially heated under pressurization and is polymerized within 5 hours, 120 DEG C 5 hours, 180 DEG C and is polymerized 5 hours, cooling obtains product.Product section is 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 2.57 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 17%.Determined by GPC, resin weight average molecular weight is obtained for 34.8 ten thousand.
Embodiment 9：Butadiene rubber after 10 grams are vacuum dried is put in 2l there-necked flasks, adds 990 grams of styrene, under agitation by butadiene rubber swelling or dissolving；Obtain thermoplastic resin composition.The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by thermoplastic resin composition's priming by vacuum of 30ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 50 DEG C of polymerase 10 .5 hours, 90 DEG C of polymerase 10 .5 hours, 120 DEG C of polymerase 10 .5 hours, 140 DEG C of polymerase 10 .5 hours, 230 DEG C of polymerase 10 .5 hours under pressurization, are sequentially heated to, cooling obtains product.Product section is 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.
Embodiment 10：Butadiene rubber after 300 grams are vacuum dried is put in 2l there-necked flasks, adds 700 grams of styrene, under agitation by butadiene rubber swelling or dissolving；Obtain thermoplastic resin composition.The carbon cloth that 4 layers are cut（25cm*25cm）It is put into mould（25cm*25cm）In, by thermoplastic resin composition's priming by vacuum of 100ml in mould, by carbon cloth thorough impregnation；Hot press is put into rear mold, 50 DEG C of polymerase 10 .5 hours, 120 DEG C of polymerase 10 .5 hours, 140 DEG C of polymerase 10 .5 hours, 230 DEG C of polymerase 10 .5 hours under pressurization, are sequentially heated to, cooling obtains product.Product section is 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.
Claims (10)
1. a kind of fibre reinforced thermoplas tic resin composite, it is characterised in that:Which includes polystyrene, unsaturated rubber and continuous carbon fibre.
2. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：Which includes the continuous carbon fibre of polystyrene, unsaturated rubber and volume content between 1%-60%.
3. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：The weight average molecular weight of the polystyrene is 30,000-50 ten thousand.
4. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：Described unsaturated rubber is one or more mixture in natural rubber, butadiene rubber, butyl rubber, butadiene-styrene rubber, nitrile rubber and neoprene.
5. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：Content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 1wt%-30wt%.
6. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：Content of the unsaturated rubber in polystyrene and unsaturated rubber total amount is 5wt%-15wt%.
7. the 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%.
8. the manufacture method of the fibre reinforced thermoplas tic resin composite as described in any one in claim 1-7, it is characterised in that：Comprise the steps
（1）Impregnation：The continuous carbon fibre of the content is immersed in resin combination, impregnation system is obtained；Polystyrene containing 0-50wt% wherein in resin combination, the unsaturated rubber of 1-30wt%, remaining is styrene monomer；
（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 add up to 2-30h.
9. the manufacture method of fibre reinforced thermoplas tic resin composite according to claim 8, it is characterised in that：Content 5-30wt% of polystyrene, unsaturated rubber content 5wt%-15wt% in described resin combination, remaining is styrene monomer.
10. the manufacture method of fibre reinforced thermoplas tic resin composite according to claim 8, it is characterised in that：Viscosity at 25 DEG C of the resin combination is 50-50000mPa*s.
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| CN114874605A (en) * | 2022-05-09 | 2022-08-09 | 上海大学 | Continuous carbon fiber reinforced thermosetting resin prepreg filament and preparation method and application thereof |
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Application publication date: 20170419 |