CN107118518A - A kind of carbon fiber prepreg and preparation method thereof - Google Patents
A kind of carbon fiber prepreg and preparation method thereof Download PDFInfo
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- CN107118518A CN107118518A CN201710550332.0A CN201710550332A CN107118518A CN 107118518 A CN107118518 A CN 107118518A CN 201710550332 A CN201710550332 A CN 201710550332A CN 107118518 A CN107118518 A CN 107118518A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Reinforced Plastic Materials (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of carbon fiber prepreg and preparation method thereof, carbon fiber prepreg is mainly composed of the following components：Epoxy resin, curing agent, accelerator and carbon fiber；The epoxy resin is 1 by mass ratio:1‑2:1 novolac epoxy resin, liquid bisphenol A epoxy resin and solid-state bisphenol A epoxide resin composition.The carbon fiber prepreg of the present invention is more than 12 months in the normal temperature storage time, can be widely applied to the fields such as fishing tackle, sports equipment, sports goods, Aero-Space.
Description
Technical field
The present invention relates to high polymer material and preparation method thereof, more particularly to a kind of carbon fiber prepreg and its preparation side
Method.
Background technology
Carbon fiber prepreg is that also have the material such as other by carbon fiber yarn, epoxy resin, by film, hot pressing, cools down, covers
Film, the composite that technique is processed, also known as the carbon fibre initial rinse fabric such as batch；Carbon fiber prepreg be widely used in fishing tackle,
The fields such as sports equipment, sports goods, Aero-Space, at present, carbon fiber prepreg longer-term storage need low-temperature storage, add it
Application cost.The prepreg that CN201310515677.4 stablizes there is provided a kind of room temperature storage, solidfied material mechanics, but it is raw at present
The normal temperature storage time of the carbon fiber prepreg of production needs further improve.In addition, improving the normal temperature storage of carbon fiber prepreg
Another difficulty of time is that the component after production difficulty increase after formula changes, adjustment formula can not realize continuous production, and raw
The material heterogeneity of production.
Applicant is directed to the research of carbon fiber prepreg always, already have carbon fiber prepreg production practices and
A kind of theoretical foundation, such as 201610338104.2 (preparation methods of high-strength carbon fiber prepreg), discloses applicant's system
Related component in standby carbon fiber prepreg, such as liquid epoxy resin, solid epoxy, curing agent and accelerator, still
Applicant still encounters following problem when the carbon fiber prepreg of normal temperature storage is capable of in research：1st, adjustment resin ratio and
During resinous type, even if the replacement of the adjustment of small range resin similar with structure, to product gel-forming property and finally after solidification
Performance impact it is very big, and adjustment after formula can not mass produce；2nd, because carbon fiber prepreg is in itself to material property
It is required that high and production technology complexity, causes applicant when adjusting its formula, to overall performance and the production week of material
Phase makes a big impact.
The content of the invention
Goal of the invention：The present invention provides a kind of carbon fiber prepreg for being capable of long-time normal temperature storage, the carbon fibre initial rinse
Expect the stable mechanical property of the solidfied material of material；It is a further object of the present invention to provide a kind of preparation side of carbon fiber prepreg
Method, simple production process.
Technical scheme：A kind of carbon fiber prepreg of the present invention, it is main composed of the following components：Epoxy resin, solidification
Agent, accelerator and carbon fiber；The epoxy resin is 1 by mass ratio:1-2:1 novolac epoxy resin, liquid bisphenol A epoxy tree
Fat and solid-state bisphenol A epoxide resin composition.
The one kind of the novolac epoxy resin in NPCN-704 or 638S.The liquid bisphenol A epoxy resin is
NPEL-128.The solid-state bisphenol A epoxide resin is NPES-901.The maximum feature of prepreg is that production difficulty is big, and its is follow-up
Laying method need compacting because of every layer, therefore operation is slow, therefore selection of the prepreg in process of production to resin binder is extremely harsh,
Gelation time and deaeration are influenceed, if Choice of Resin is improper, gummosis can be also caused during production, the product thickness of production is caused not
It is homogeneous.
The curing agent quality is 3-8 with epoxy resin mass ratio:100.Curing agent reacts with epoxy resin, is formed
Netted space polymers, the mechanical property of the selection influence final material of curing agent.
The accelerator quality is 0.5-5 with epoxy resin and curing agent total mass ratio:100.Accelerator can improve instead
Speed is answered, but its consumption in the product is less.The present invention curing agent and accelerator combination, do not require nothing more than its at normal temperatures with
Resin material is mixed well, and the stabilization of material is not influenceed in long-term normal temperature storing process, also requires that it keeps activity, in material
During solidification, the curing materials of excellent in mechanical performance are obtained.Further, since the requirement of process for manufacturing prepregs, epoxy resin, solidification
The system of agent and accelerator need to not influence follow-up production technology.
The carbon fiber quality is 1-4 with epoxy resin, curing agent and accelerator total mass ratio:1.
The one kind of the curing agent in dicyandiamide 100S, 100SF or DDA-5.
The one kind of the accelerator in ureas UR700, modified imidazole PN40 or modified imidazole PN50.
One or more of the carbon fiber in 45S, M30 or M40.
The preparation method of above-mentioned carbon fiber prepreg, it is characterised in that comprise the following steps：(1) by novolac epoxy resin,
Liquid bisphenol A epoxy resin and solid-state bisphenol A epoxide resin are stirred at 80-90 DEG C, after mixing completely, obtain mixed liquor A；
(2) curing agent is added in the mixed liquor A obtained to step (1), after being stirred at 70-80 DEG C, obtains mixed liquid B；(3) to
Accelerator is added in the mixed liquid B that step (2) is obtained, after being stirred at 70-80 DEG C, mixed liquor C is obtained；(4) will be above-mentioned
Mixed liquor C obtains glued membrane through gluing, and glued membrane and carbon fiber are obtained into carbon fiber prepreg by preimpregnated process processing.The carbon of preparation is fine
Prepreg is tieed up in normal temperature storage, surface viscosity does not change, then material belongs to stable state at normal temperatures.
Wherein, when mixed liquor C viscosity is relatively low, then before gluing, primary solidification is needed, gluing is then carried out again, the present invention
In order to reduce curing schedule, adjustment mixed liquor C viscositys are 10000-60000cps.The viscosity is normal in normal temperature by Brookfield viscometer
Pressure is determined.By resin, curing agent and the selection of accelerator, mixed liquor C is in the range of the viscosity, without solidifying and reducing
The time of coating film forming in production process, carbon fiber prepreg viscosity is controlled in addition, the deaeration solved in production process is stranded
It is difficult.
The gluing verifies the grammes per square metre of every square meter of glued membrane, reduced by coldplate for mixed liquor C is placed in glue spreader
The temperature of glued membrane obtains glued membrane to normal temperature.The preimpregnated process is that glued membrane is drawn from the upper and lower glued membrane roller of prepreg machine, and and carbon
Fiber formation sandwich structure, passes sequentially through hot-pressing roller, melts resin matrix, in carbon fiber embedded resin matrix, cooling reduction
Prepreg temperature is to normal temperature.
Beneficial effect：The carbon fiber prepreg of the present invention can be more than 12 months the normal temperature storage time, and product mechanical property
Can be excellent；Carbon fiber prepreg production craft step prepared by the present invention is simple, and temperature control is suitable in production process, Bu Huizao
Into product high temperature deformation.
Embodiment
First, raw material sources
1st, novolac epoxy resin is purchased from NPCN-704 the or 638S epoxy novolac trees that South Asia epoxy resin Co., Ltd produces
Fat；Liquid bisphenol A epoxy resin is purchased from the NPEL-128 that South Asia epoxy resin Co., Ltd produces；Solid-state bisphenol A epoxide resin
The NPES-901 produced purchased from South Asia epoxy resin Co., Ltd；
2nd, carbon fiber 45S, M30 or M40 is purchased from Zhongfu Shenying Carbon Fiber Limited Liability Company；
3rd, curing agent dicyandiamide 100S, dicyandiamide 100SF and dicyandiamide DDA-5 are purchased from German goldschmidt chemical corporation；
4th, accelerator ureas UR700 is purchased from German goldschmidt chemical corporation；Modified imidazole PN40 and PN50 is fine purchased from aginomoto
KCC；
5th, remaining material gained purchased in market.
2nd, properties of sample is detected
1st, properties of sample is tested：Reference《GB/T 2567-2008 casting resin method for testing performances》.
3rd, sample preparation
Embodiment 1：By novolac epoxy resin NPCN-704, liquid bisphenol A epoxy resin NPEL-128 and solid-state bisphenol-A ring
Each 10kg of oxygen tree fat NPES-901 are stirred at 80 DEG C, after mixing completely, obtain mixed liquor A；0.9kg is added into mixed liquor A
Curing agent dicyandiamide 100S, after being stirred at 70 DEG C, obtains mixed liquid B, and 0.15kg accelerator is added into mixed liquid B
UR700, after being stirred at 70 DEG C, obtains mixed liquor C, mixed liquor C viscositys are 10000cps, take 2kg mixed liquors C in 150
DEG C solidification 2h, obtains epoxy resin casting matrix, determines epoxy resin casting matrix performance.Residual mixed liquor C is placed in glue spreader, led to
Cross infrared ray instrument verification glued membrane per square meter grammes per square metre, by coldplate reduce glued membrane temperature to normal temperature, obtain glued membrane, by glued membrane from
Drawn in the upper and lower glued membrane roller of prepreg machine, and pass sequentially through hot-pressing roller into sandwich structure with 31kg carbon fibers 45S, make resin base
Body is melted, in carbon fiber embedded resin matrix, and cooling reduction prepreg temperature to normal temperature processing obtains carbon fiber prepreg.
Embodiment 2：10kg novolac epoxy resin 638S, 20kg liquid bisphenol A epoxy resins NPEL-128 and 10kg are consolidated
State bisphenol A epoxide resin NPES-901 is stirred at 90 DEG C, after mixing completely, obtains mixed liquor A；Added into mixed liquor A
1.5kg curing agent dicyandiamide 100SF, after being stirred at 80 DEG C, obtain mixed liquid B, and 0.83kg is added into mixed liquid B and is promoted
Enter agent modified imidazole PN40, after being stirred at 80 DEG C, obtain mixed liquor C, mixed liquor C viscositys are 20000cps, take 2kg to mix
Close liquid C and solidify 2h in 150 DEG C, obtain epoxy resin casting matrix, determine epoxy resin casting matrix performance.Residual mixed liquor C is placed in
In glue spreader, grammes per square metre of the glued membrane per square meter is verified by infrared ray instrument, the temperature for reducing glued membrane by coldplate obtains glue to normal temperature
Film, glued membrane is drawn from the upper and lower glued membrane roller of prepreg machine, and forms sandwich structure with 85kg carbon fibers M30, passes sequentially through heat
Pressure roller, melts resin matrix, in carbon fiber embedded resin matrix, and it is fine that cooling reduction prepreg temperature to normal temperature processing obtains carbon
Tie up prepreg.
Embodiment 3：10kg novolac epoxy resin 638S, 15kg liquid bisphenol A epoxy resins NPEL-128 and 10kg are consolidated
State bisphenol A epoxide resin NPES-901 is stirred at 85 DEG C, after mixing completely, obtains mixed liquor A；Added into mixed liquor A
2.8kg curing agent dicyandiamide DDA-5, after being stirred at 75 DEG C, obtain mixed liquid B, and 1.1kg is added into mixed liquid B and is promoted
Enter agent modified imidazole PN50, after being stirred at 75 DEG C, obtain mixed liquor C, mixed liquor C viscositys are 40000cps, take 2kg to mix
Close liquid C and solidify 2h in 150 DEG C, obtain epoxy resin casting matrix, determine epoxy resin casting matrix performance.Residual mixed liquor C is placed in
In glue spreader, grammes per square metre of the glued membrane per square meter is verified by infrared ray instrument, the temperature for reducing glued membrane by coldplate obtains glue to normal temperature
Film, glued membrane is drawn from the upper and lower glued membrane roller of prepreg machine, and forms sandwich structure with 116.8kg carbon fibers M40, is led to successively
Hot-pressing roller is crossed, resin matrix is melted, in carbon fiber embedded resin matrix, cooling reduction prepreg temperature to normal temperature processing is obtained
Carbon fiber prepreg.
Embodiment 4：The NPEL- that NPCN-704 that novolac epoxy resin is 10kg, liquid bisphenol A epoxy resin are 10kg
128 and solid-state bisphenol A epoxide resin be 10kg NPES-901, curing agent be 1.8kg dicyandiamide 100SF, accelerator is 1.5kg
Ureas UR700, mixed liquor C viscosity are 60000cps, and carbon fiber is 133.5kg M30, remaining be the same as Example 3.
Embodiment 5：The NPEL- that NPCN-704 that novolac epoxy resin is 10kg, liquid bisphenol A epoxy resin are 20kg
128 and solid-state bisphenol A epoxide resin be 10kg NPES-901, curing agent be 2kg dicyandiamide 100S, accelerator be 1.3kg ureas
Class UR700, mixed liquor C viscosity are 40000cps, and carbon fiber is 129.8kg 45S, remaining be the same as Example 3.
Comparative example 1：Epoxy resin is 17.5kg novolac epoxy resin 638S and 17.5kg solid-state bisphenol A epoxide resins
NPES-901, residual mixed liquor C is solidified 30 minutes at 80 DEG C, is placed in glue spreader, remaining be the same as Example 3.
Comparative example 2：Epoxy resin is 21kg liquid bisphenol A epoxy resin NPEL-128 and 14kg solid-state bisphenol-A asphalt mixtures modified by epoxy resin
Fat NPES-901, residual mixed liquor C is solidified 30 minutes at 80 DEG C, is placed in glue spreader, remaining be the same as Example 3.
Comparative example 3：Curing agent is dicyandiamide 1400F in raw material, and residual mixed liquor C is solidified 50 minutes at 80 DEG C, is placed in
In glue spreader, remaining be the same as Example 3.
Comparative example 4：Accelerator is substituted urea UR-D in raw material, and residual mixed liquor C is solidified 50 minutes at 80 DEG C, painting is placed in
In glue machine, remaining be the same as Example 3.
Comparative example 5：Curing agent is that dicyandiamide 1400F, accelerator are substituted urea UR-D in raw material, and residual mixed liquor C is existed
80 DEG C solidify 60 minutes, are placed in glue spreader, remaining be the same as Example 3.
4th, result is determined
The properties of sample measurement result of table 1
Sample stores surface after 12 months and does not occur any change at normal temperatures it can be seen from the result of table 1, and sample is solid
Excellent in mechanical performance after change, can be applied in different fields.
Claims (10)
1. a kind of carbon fiber prepreg, it is characterised in that main composed of the following components：Epoxy resin, curing agent, accelerator and
Carbon fiber；The epoxy resin is 1 by mass ratio:1-2:1 novolac epoxy resin, liquid bisphenol A epoxy resin and Solid Double
Phenol A epoxy resin is constituted.
2. carbon fiber prepreg according to claim 1, it is characterised in that the curing agent is with epoxy resin mass ratio
3-8:100。
3. carbon fiber prepreg according to claim 1, it is characterised in that the consumption of the accelerator is and epoxy resin
It is 0.5-5 with curing agent total mass ratio:100.
4. carbon fiber prepreg according to claim 1, it is characterised in that the consumption of the carbon fiber be with epoxy resin,
Curing agent and the total mass ratio of accelerator are 1-4:1.
5. carbon fiber prepreg according to claim 1, it is characterised in that the novolac epoxy resin is selected from NPCN-704
Or one kind in 638S.
6. carbon fiber prepreg according to claim 1, it is characterised in that the curing agent be selected from dicyandiamide 100S,
One kind in 100SF or DDA-5.
7. carbon fiber prepreg according to claim 1, it is characterised in that the accelerator is selected from ureas UR700, modification
One kind in imidazoles PN40 or modified imidazole PN50.
8. carbon fiber prepreg according to claim 1, it is characterised in that the carbon fiber is in 45S, M30 or M40
One or more.
9. the preparation method of the carbon fiber prepreg described in a kind of claim 1-8, it is characterised in that comprise the following steps：
(1) novolac epoxy resin, liquid bisphenol A epoxy resin and solid-state bisphenol A epoxide resin are stirred at 80-90 DEG C, mixed
After closing completely, mixed liquor A is obtained；
(2) curing agent is added in the mixed liquor A obtained to step (1), after being stirred at 70-80 DEG C, obtains mixed liquid B；
(3) accelerator is added in the mixed liquid B obtained to step (2), after being stirred at 70-80 DEG C, obtains mixed liquor C；
(4) above-mentioned mixed liquor C is obtained into glued membrane through gluing, glued membrane and carbon fiber is obtained into carbon fibre initial rinse by preimpregnated process processing
Material.
10. the preparation method of carbon fiber prepreg according to claim 9, it is characterised in that in step (3), the mixing
Liquid C viscositys are 10000-60000cps.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710550332.0A CN107118518A (en) | 2017-07-07 | 2017-07-07 | A kind of carbon fiber prepreg and preparation method thereof |
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| CN201710550332.0A CN107118518A (en) | 2017-07-07 | 2017-07-07 | A kind of carbon fiber prepreg and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107538770A (en) * | 2017-09-28 | 2018-01-05 | 国营芜湖机械厂 | A kind of advanced composite material repairing material and repair method |
| CN107964217A (en) * | 2017-12-14 | 2018-04-27 | 郑州四维特种材料有限责任公司 | A kind of carbon fibre reinforced composite resin matrix, carbon fibre reinforced composite and preparation method thereof, base plate of ping-pong bat |
| CN108641287A (en) * | 2018-04-13 | 2018-10-12 | 航天材料及工艺研究所 | A kind of epoxy-resin systems, preparation method and prepreg |
| CN109608825A (en) * | 2018-11-30 | 2019-04-12 | 中国航空工业集团公司基础技术研究院 | A kind of sacrificial layer Ultraluminescence epoxy resin carbon fiber prepreg |
| CN113278180A (en) * | 2021-05-21 | 2021-08-20 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy carbon fiber insulating layer, molded part and preparation method thereof |
| CN113278179A (en) * | 2021-05-21 | 2021-08-20 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy glass fiber insulating layer, molded part and preparation method thereof |
| CN116751439A (en) * | 2023-08-21 | 2023-09-15 | 山东天迈化工有限公司 | Epoxy resin, production method thereof and epoxy resin prepreg |
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| CN103396656A (en) * | 2013-08-27 | 2013-11-20 | 连云港神鹰碳纤维自行车有限责任公司 | Preparation method of epoxy resin system for nanometer modified carbon fiber prepreg |
| CN105968731A (en) * | 2016-05-27 | 2016-09-28 | 江苏兆鋆新材料股份有限公司 | Low-temperature curing epoxy resin carbon fiber prepreg and preparing method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107538770A (en) * | 2017-09-28 | 2018-01-05 | 国营芜湖机械厂 | A kind of advanced composite material repairing material and repair method |
| CN107964217A (en) * | 2017-12-14 | 2018-04-27 | 郑州四维特种材料有限责任公司 | A kind of carbon fibre reinforced composite resin matrix, carbon fibre reinforced composite and preparation method thereof, base plate of ping-pong bat |
| CN108641287A (en) * | 2018-04-13 | 2018-10-12 | 航天材料及工艺研究所 | A kind of epoxy-resin systems, preparation method and prepreg |
| CN109608825A (en) * | 2018-11-30 | 2019-04-12 | 中国航空工业集团公司基础技术研究院 | A kind of sacrificial layer Ultraluminescence epoxy resin carbon fiber prepreg |
| CN113278180A (en) * | 2021-05-21 | 2021-08-20 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy carbon fiber insulating layer, molded part and preparation method thereof |
| CN113278179A (en) * | 2021-05-21 | 2021-08-20 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy glass fiber insulating layer, molded part and preparation method thereof |
| CN113278179B (en) * | 2021-05-21 | 2022-08-12 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy glass fiber insulating layer, molded part and preparation method thereof |
| CN113278180B (en) * | 2021-05-21 | 2022-08-12 | 四川东材科技集团股份有限公司 | High-temperature-resistance epoxy carbon fiber insulating layer, molded part and preparation method thereof |
| CN116751439A (en) * | 2023-08-21 | 2023-09-15 | 山东天迈化工有限公司 | Epoxy resin, production method thereof and epoxy resin prepreg |
| CN116751439B (en) * | 2023-08-21 | 2023-12-29 | 山东天迈化工有限公司 | Epoxy resin, production method thereof and epoxy resin prepreg |
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Application publication date: 20170901 |