CN106566098A - 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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- CN106566098A CN106566098A CN201510638644.8A CN201510638644A CN106566098A CN 106566098 A CN106566098 A CN 106566098A CN 201510638644 A CN201510638644 A CN 201510638644A CN 106566098 A CN106566098 A CN 106566098A
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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 comprises polystyrene and continuous carbon fibers. The preparation method comprises impregnation and in-situ polymerization. Impregnation refers to impregnation of the continuous carbon fibers in a resin composition, wherein the resin composition contains 5 to 30 wt% of polystyrene and 95 to 70 wt% of a styrene monomer and forms an impregnation system; and in-situ polymerization refers to polymerization in the impregnation system at 60 to 180 DEG C for 2 to 20 h. The carbon fiber-reinforced thermoplastic resin composite material is uniform in structure and low in cost. The preparation method is low in preparation cost, suitable for large-scale production; and the prepared composite material has a uniform structure, does not use any solvent and presents good thermoplastic molding performance.
Description
Technical field
The present invention relates to fibre reinforced thermoplas tic resin composite and preparation method thereof.
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 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 and continuous carbon fibre.
Which includes the continuous carbon fibre of polystyrene and volume content for 1%-60%.
The molecular weight of the polystyrene is 30,000-50 ten thousand.The too low mechanical property for then affecting composite of molecular weight of polystyrene, the too high processing for then affecting composite.It is 80,000-50 ten thousand as the molecular weight of preferred polystyrene, optimum is 100,000-40 ten thousand.
Preferably, the volume content of the continuous carbon fibre is 10-50%.
Used as further 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.
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 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；Polystyrene containing 1-50wt% wherein in resin combination, remaining is styrene monomer；
（2）In-situ polymerization：By step（1）Impregnation system in the 50-230 DEG C of temperature range zone heating from low to high, be polymerized, polymerization time adds up to 2-30h.
In resin combination, the content of polystyrene is 5-35wt%, and remaining is styrene monomer.
Content 10-30wt% of polystyrene, remaining is styrene monomer.
Viscosity at 25 DEG C of the resin combination is between 50-50000mPa*s.
Viscosity at 25 DEG C of the resin combination is between 100-50000mPa*s.
Viscosity at 25 DEG C of the resin combination is between 500-50000mPa*s.
Impregnation refers to and continuous carbon fibre is immersed in resin combination, the resin combination is the compositionss of polystyrene and styrene monomer, in view of resin combination viscosity to be impregnated with performance impact, for the impregnation for having reached, resin combination is in 25 DEG C of viscosity with 500-50000mPa*s as optimum.
Preferably, in-situ polymerization temperature range is 60-200 DEG C.
As further, preferably, in-situ polymerization temperature range is 60-180 DEG C, and polymerization time adds up to 2-20h.
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.Polymerization temperature interval is advisable with 50-230 DEG C, can be optimized for 60-200 DEG C, can be further optimized for 60-180 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, polymerization time is total can be optimized for 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, the good product quality and steady quality after molding, the composite conjugation obtained by copolyreaction are high, uniform in material, the strength of materials are high.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, materials described below has been used as raw material：
Styrene monomer, 99%, the tert-butyl catechol stabilizers of 4- containing 10-15ppm, purchased from Shanghai Aladdin biochemical technology limited company；
Carbon cloth, YT-3K-X200, purchased from Yixing City Yi Tai carbon fiber weavings company limited.
It is prepared by thermoplastic resin composition
Embodiment 1：Under nitrogen protection 1000ml styrene is added in 2l there-necked flasks, Jing after nitrogen displacement 3 times, system 80 DEG C is heated under nitrogen atmosphere, now polymerization starts.Be polymerized after 5% being reached to styrene conversion rate, system is dropped to rapidly room temperature, thermoplastic resin composition A is obtained.
Embodiment 2：Under nitrogen protection 1000ml styrene is added in 2l there-necked flasks, Jing after nitrogen displacement 3 times, system 80 DEG C is heated 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：Under nitrogen protection 1000ml styrene is added in 2l there-necked flasks, Jing after nitrogen displacement 3 times, system 80 DEG C is heated 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：Under nitrogen protection 1000ml styrene is added in 2l there-necked flasks, Jing after nitrogen displacement 3 times, system 80 DEG C is heated 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 6.66 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 54%.Determined by GPC, resin weight average molecular weight is obtained for 7.3 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 5.91 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 46%.Determined by GPC, resin weight average molecular weight is obtained for 9.8 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 4.32 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 31%.Determined by GPC, resin weight average molecular weight is obtained for 16.9 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 2.30 grams of carbon cloths, can estimate that from it volume content of carbon fiber is 15%.Determined by GPC, resin weight average molecular weight is obtained for 37.6 ten thousand.
Claims (10)
1. a kind of fibre reinforced thermoplas tic resin composite, it is characterised in that：Which includes polystyrene 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 and volume content for 1%-60%.
3. the fibre reinforced thermoplas tic resin composite according to claim 1, it is characterised in that：The 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：The volume content of the continuous carbon fibre is 10-50%.
5. 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 20-50%.
6. the preparation method of the fibre reinforced thermoplas tic resin composite such as claim 1-5 as described in any one, it is characterised in that comprise the steps：
（1）Impregnation：Continuous carbon fibre is immersed in resin combination, impregnation system is obtained；Polystyrene containing 1-50wt% wherein in resin combination, remaining is styrene monomer；
（2）In-situ polymerization：By step（1）The impregnation system for obtaining zone heating from low to high in the 50-230 DEG C of temperature range, is polymerized, and 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：In resin combination, the content of polystyrene is 5-35wt%, and remaining is styrene monomer.
8. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：Content 10-30wt% of polystyrene, remaining is styrene monomer.
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 between 50-50000mPa*s.
10. the preparation method of fibre reinforced thermoplas tic resin composite according to claim 6, it is characterised in that：In-situ polymerization temperature range is 60-200 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107856325A (en) * | 2017-12-07 | 2018-03-30 | 武汉纺织大学 | One kind is used for continuous fiber reinforced thermoplastic matrix composite and preparation method |
| CN108125713A (en) * | 2017-12-28 | 2018-06-08 | 武汉康斯泰德科技有限公司 | Long-chain carbon fiber PEEK outer wrapping thermoforming bone fixation plates and forming method |
-
2015
- 2015-10-08 CN CN201510638644.8A patent/CN106566098A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107856325A (en) * | 2017-12-07 | 2018-03-30 | 武汉纺织大学 | One kind is used for continuous fiber reinforced thermoplastic matrix composite and preparation method |
| CN108125713A (en) * | 2017-12-28 | 2018-06-08 | 武汉康斯泰德科技有限公司 | Long-chain carbon fiber PEEK outer wrapping thermoforming bone fixation plates and forming method |
| CN108125713B (en) * | 2017-12-28 | 2024-02-23 | 武汉康斯泰德科技有限公司 | Long-chain carbon fiber PEEK (polyether-ether-ketone) outer-wrapped thermal-forming bone fixing plate and forming method |
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