CN104002523B - Flame retardant carbon fiber prepreg and preparation method thereof - Google Patents
Flame retardant carbon fiber prepreg and preparation method thereof Download PDFInfo
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- CN104002523B CN104002523B CN201410157894.5A CN201410157894A CN104002523B CN 104002523 B CN104002523 B CN 104002523B CN 201410157894 A CN201410157894 A CN 201410157894A CN 104002523 B CN104002523 B CN 104002523B
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Abstract
The invention discloses a flame retardant carbon fiber prepreg, which includes a carbon fiber layer and flame retardant epoxy resin impregnated in the carbon fiber layer; and release paper directly attached to the outer surface of the carbon fiber layer. In addition, the invention also discloses a hot melting two-step preparation method for the carbon fiber prepreg, and the method includes membrane preparation and preimpregnation. The method provided by the invention is simple, the prepared flame retardant carbon fiber prepreg can have a very good flame retardant effect, and at the same time, the product also meets the demands (ROSH, Reach up to stand) of environmental protection products. Thus, the flame retardant carbon fiber prepreg can be widely used in the electronics and other 3C product field so as to form lightweight, high strength and flame retardant carbon fiber products.
Description
Technical field
The present invention relates to carbon fiber prepreg, more particularly to a kind of carbon fiber prepreg with flame retardant effect.
Background technology
Carbon fiber is national economy and the indispensable strategic new material of national defense construction, is that advanced composite material is most important
One of reinforcement, it has, and intensity is high, density is little, and plasticity is strong, the advantages of corrosion-resistant, life-span length, is therefore widely used in
The fields such as Aero-Space, resource equipment, transportation, architectural engineering, Leisure Sport.In prior art, carbon fiber prepreg is equal
It is the carbon fiber layer being soaked with conventional epoxy, because conventional epoxy does not have anti-flammability, carbon therefore of the prior art
Fiber prepreg material may not apply on electronics 3c product.
Content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of dipping fire retarding epoxide resin have fire-retardant
The carbon fiber prepreg of effect, and present invention also offers the preparation method of this carbon fiber prepreg.
To achieve these goals, the technical scheme that the present invention takes is as follows:
A kind of fire-retardant carbon fiber prepreg, including carbon fiber layer and be immersed in fire retarding epoxide resin therein, also includes straight
Connect note and invest the release paper on carbon fiber layer outer surface.
Further, the fiber in described carbon fiber layer is that same direction parallel arranged group sets and forms, between carbon fiber
Mutually impregnated using fire retarding epoxide resin.
A kind of hot melt two step method preparation method of described carbon fiber prepreg, including masking and preimpregnation.
Further, described masking comprises the following steps:
1) flame-retarded resin matrix is placed in blender and is sufficiently mixed；
2) after rubber roll is heated to 70 DEG C, it is transported to glue spreader, adjust the spacing of glue spreader and the operation linear speed of release paper
Degree, the glued membrane of prepared different-thickness；
3) use the infrared ray instrument detection thickness of glued membrane or the surface density of glued membrane, reduce the temperature of glued membrane by coldplate, subtract
Its state of cure few；
4) winding, packaging, deposit in freezer stand-by.
Further, described flame-retarded resin is grouped into by the group of following weight ratio:
Atn series epoxy resins: 12-15%；E-51:15-20%；E-44:5-8%；E-20:40-45%；The double cyanogen of micronization
Amine: 5-8%；Ureas accelerator: 1-1.5%；Hydrated alumina: 10-15%；White carbon thickening agent: 0.5-1%.
Further, described flame-retarded resin is obtained by following steps:
1) epoxy resin is put in 100～150 DEG C of baking oven and preheat 7～9 hours, remove moisture and little volatilization in resin
Divide material；
2) weigh a small amount of liquid epoxies respectively to put in dough batch in advance with quantitative firming agent, accelerator, fire retardant
First mix, stir 20～40min, be respectively prepared firming agent and accelerator and flame retardant resin paste；
3) resin paste that step 2 is obtained is ground two to three times on three-roll grinder, and it is less to obtain viscosity, powder diameter
More uniform firming agent and accelerator and flame retardant masterbatch；
4) epoxy resin of preheating is put into stirring in reactor, and froth in vacuum, cool to 80 DEG C simultaneously；
5) treat that resin temperature drops to 70～75 DEG C, be separately added into ground firming agent and accelerator and fire retardant is female
Material, mixes 20～30 minutes in reactor high speed, powerful vacuum removes bubble removing simultaneously；
6) mixed resin is separately flowed into pallet under swager effect, by mono- piece of segmentation of 5kg, naturally cold at room temperature
But, after, by 6 pieces of a carton (30kg) packaging, obtain prepreg fire retarding epoxide resin system finished product.
Further, described preimpregnation comprises the following steps:
1) draw fiber from creel, after regulation tension force, collection filament plate boundling, flattening process, reach the width of regulation；
2) draw ready made glued membrane from upper and lower glued membrane roller, and form sandwich structure with fiber, pass sequentially through several groups of heat
Pressure roller, makes resin matrix melt, in fiber embedded resin matrix；
3) cooling reduces prepreg temperature；
4) finally carry out trimming, cover pe film, winding, fire-retardant prepreg is obtained.
The present invention increased the flame retardant effect of carbon fiber prepreg under the premise of not changing current initial rinsing method, overcomes mesh
On front market, the non-antiflaming effect of carbon fiber prepreg of circulation is it is impossible to using the problem in related special dimension, widen carbon fine
The range of application of fiber products, simultaneously the present invention by fire retarding epoxide resin presoak carbon fiber by way of obtain carbon fiber prepreg,
Method is simple, and the product of production process and acquisition is satisfied by environment-friendly products and requires (rosh, reach are all qualified).The carbon of the present invention
Fiber prepreg material can be widely used in the 3c product scope such as electronics, forms light weight, intensity is higher and has flame retardant effect
Carbon fiber product.
Brief description
Fig. 1 is the flow chart of the film making process of the present invention；
Fig. 2 is the flow chart of the preimpregnation operation of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with the accompanying drawings and embodiment, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, not
For limiting the present invention.
The fire-retardant carbon fiber prepreg of the present invention, including carbon fiber layer and be immersed in fire retarding epoxide resin therein, and
Directly note invests the release paper on carbon fiber layer outer surface.Fiber in described carbon fiber layer is that same direction parallel arranged group sets
, mutually impregnated using fire retarding epoxide resin between carbon fiber.
The carbon fiber prepreg of the present invention is prepared by hot melt two step method, and this preparation method includes masking and preimpregnation.Masking
Including step: 1) fire retarding epoxide resin matrix is placed in blender and is sufficiently mixed；2) after rubber roll is heated to 70 DEG C, conveying
To glue spreader, adjust the spacing of glue spreader and the operation linear velocity of release paper, the glued membrane of prepared different-thickness；3) use infrared ray instrument
The detection thickness of glued membrane or the surface density of glued membrane, are reduced the temperature of glued membrane, reduce its state of cure by coldplate；4) wind,
Packaging, deposits in freezer stand-by.Preimpregnation includes step: 1) draws fiber from creel, by adjusting tension force, collection filament plate boundling, exhibition
After flat program, reach the width of regulation；2) draw ready made glued membrane from upper and lower glued membrane roller, and form sandwich and tie with fiber
Structure, passes sequentially through several groups of hot-pressing rollers, so that resin matrix is melted, in fiber embedded resin matrix；3) cooling reduces prepreg temperature；
4) finally carry out trimming, cover pe film, winding, fire-retardant prepreg is obtained.
The preparation of the fire retarding epoxide resin of the fire-retardant carbon fiber prepreg of the present invention is now illustrated by following examples
Journey.
Embodiment 1
Described flame-retarded resin is grouped into by the group of following weight ratio:
Atn series epoxy resins: 12%；E-51:17%；E-44:6%；E-20:43%；Micronization dicyandiamide: 5%；Ureas promotees
Enter agent: 1.5%；Hydrated alumina: 15%；White carbon thickening agent: 0.5%.
1) epoxy resin is put in 110 DEG C of baking oven and preheat 7 hours, remove moisture and little volatile matters material in resin；
2) weigh a small amount of liquid epoxies respectively to put in dough batch in advance with quantitative firming agent, accelerator, fire retardant
First mix, stir 25min, be respectively prepared firming agent and accelerator and flame retardant resin paste；
3) resin paste that step 2 is obtained is ground two to three times on three-roll grinder, and it is less to obtain viscosity, powder diameter
More uniform firming agent and accelerator and flame retardant masterbatch；
4) epoxy resin of preheating is put into stirring in reactor, and froth in vacuum, cool to 80 DEG C simultaneously；
5) treat that resin temperature drops to 70 DEG C, be separately added into ground firming agent and accelerator and flame retardant masterbatch,
Mix 20 minutes in reactor high speed, powerful vacuum removes bubble removing simultaneously；
6) mixed resin is separately flowed into pallet under swager effect, by mono- piece of segmentation of 5kg, natural at room temperature
After cooling, by 6 pieces of a carton (30kg) packaging, obtain prepreg fire retarding epoxide resin system finished product.
Embodiment 2
Described flame-retarded resin is grouped into by the group of following weight ratio:
Atn series epoxy resins: 13%；E-51:19%；E-44:5%；E-20:45%；Micronization dicyandiamide: 6%；Ureas promotees
Enter agent: 1%；Hydrated alumina: 10%；White carbon thickening agent: 1%.
1) epoxy resin is put in 120 DEG C of baking oven and preheat 8 hours, remove moisture and little volatile matters material in resin；
2) weigh a small amount of liquid epoxies respectively to put in dough batch in advance with quantitative firming agent, accelerator, fire retardant
First mix, stir 30min, be respectively prepared firming agent and accelerator and flame retardant resin paste；
3) resin paste that step 2 is obtained is ground two to three times on three-roll grinder, and it is less to obtain viscosity, powder diameter
More uniform firming agent and accelerator and flame retardant masterbatch；
4) epoxy resin of preheating is put into stirring in reactor, and froth in vacuum, cool to 80 DEG C simultaneously；
5) treat that resin temperature drops to 75 DEG C, be separately added into ground firming agent and accelerator and flame retardant masterbatch,
Mix 30 minutes in reactor high speed, powerful vacuum removes bubble removing simultaneously；
6) mixed resin is separately flowed into pallet under swager effect, by mono- piece of segmentation of 5kg, naturally cold at room temperature
But, after, by 6 pieces of a carton (30kg) packaging, obtain prepreg fire retarding epoxide resin system finished product.
Embodiment 3
Described flame-retarded resin is grouped into by the group of following weight ratio:
Atn series epoxy resins: 15%；E-51:20%；E-44:5%；E-20:40%；Micronization dicyandiamide: 8%；Ureas promotees
Enter agent: 1%；Hydrated alumina: 10%；White carbon thickening agent: 1%.
1) epoxy resin is put in 150 DEG C of baking oven and preheat 9 hours, remove moisture and little volatile matters material in resin；
2) weigh a small amount of liquid epoxies respectively to put in dough batch in advance with quantitative firming agent, accelerator, fire retardant
First mix, stir 40min, be respectively prepared firming agent and accelerator and flame retardant resin paste；
3) resin paste that step 2 is obtained is ground two to three times on three-roll grinder, and it is less to obtain viscosity, powder diameter
More uniform firming agent and accelerator and flame retardant masterbatch；
4) epoxy resin of preheating is put into stirring in reactor, and froth in vacuum, cool to 80 DEG C simultaneously；
5) treat that resin temperature drops to 73 DEG C, be separately added into ground firming agent and accelerator and flame retardant masterbatch,
Mix 25 minutes in reactor high speed, powerful vacuum removes bubble removing simultaneously；
6) mixed resin is separately flowed into pallet under swager effect, by mono- piece of segmentation of 5kg, naturally cold at room temperature
But, after, by 6 pieces of a carton (30kg) packaging, obtain prepreg fire retarding epoxide resin system finished product.
The resin that above example is obtained carries out anti-flammability test, and test equipment is: horizontal vertical combustion test instrument,
Model: rh-6033b；Test temperature: 22.5 DEG C, humidity: 51%rh；Reference standard: ul94-2013 equipment and device component are with moulding
The flammability test of material material；Testing process: setting instrument parameter → test；Sample size: 130mm × 13mm × 1mm；Sample
Pretreatment: at 23 ± 2 DEG C, 50 ± 5%rh environmental condition places 48h.
Testing procedure: flame height 20 ± 1mm, Bunsen burner is placed in center position below sample, and the Bunsen burner mouth of pipe is away from sample
Product bottom 10 ± 1mm, the duration of ignition is 10 ± 0.5s, removes Bunsen burner extremely with the speed of 300mm/sec after igniting 10 ± 0.5s
Few 150mm, starts simultaneously at record residual flame time t1, and residual flame should light 10 ± 0.5s immediately when stopping, after igniting 10 ± 0.5s with
The speed of 300mm/sec removes Bunsen burner at least 150mm, records residual flame time t2 and Yu Ran time t3 simultaneously.
Judgment criteria:
According to above step and judgment criteria, arbitrarily choose 5 from the product that described three embodiments are obtained and surveyed
Examination is simultaneously compared with usual resins, and test result is as follows:
Ul94-v1 is met by the fire retarding epoxide resin used in the present invention that relatively can be seen that of above test result
Flame-retardancy requirements.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to these embodiments, in the present invention
Application range in can carry out various changes.Although simply illustrating the preferred embodiments of the present invention above, institute
Belong to those skilled in the art and will be apparent that substantially in the range of the novelty without departing from the present invention and advantage, can be to showing
Example property embodiment carries out various modifications.
Claims (5)
1. a kind of fire-retardant carbon fiber prepreg is it is characterised in that include carbon fiber layer and fire retarding epoxide resin, wherein flame retardant epoxy
Resin is immersed in carbon fiber layer；And directly note invests the release paper on carbon fiber layer outer surface；Wherein
Described flame-retarded resin is grouped into by the group of following weight ratio: atn series epoxy resins: 12～15%；E-51:15～
20%；E-44:5～8%；E-20:40～45%；Micronization dicyandiamide: 5～8%；Ureas accelerator: 1～1.5%；Hydration oxygen
Change aluminum: 10～15%；White carbon thickening agent: 0.5～1%.
2. fire-retardant carbon fiber prepreg according to claim 1 is it is characterised in that the fiber in described carbon fiber layer is same
One direction parallel arranged group sets, and is mutually impregnated using fire retarding epoxide resin between carbon fiber.
3. a kind of hot melt two step method preparation method of the carbon fiber prepreg described in claim 1 is it is characterised in that include masking
And preimpregnation；Wherein said masking comprises the following steps:
1) flame-retarded resin matrix is placed in blender and is sufficiently mixed；
2) after rubber roll is heated to 70 DEG C, it is transported to glue spreader, adjust the spacing of glue spreader and the operation linear velocity of release paper, system
Obtain the glued membrane of different-thickness；
3) use the infrared ray instrument detection thickness of glued membrane or the surface density of glued membrane, reduce the temperature of glued membrane by coldplate, reduce it
State of cure；
4) winding, packaging, deposit in freezer stand-by；
Wherein, described flame-retarded resin is grouped into by the group of following weight ratio:
Atn series epoxy resins: 12～15%；E-51:15～20%；E-44:5～8%；E-20:40～45%；Micronization is double
Cyanamide: 5～8%；Ureas accelerator: 1～1.5%；Hydrated alumina: 10～15%；White carbon thickening agent: 0.5～1%.
4. method according to claim 3 is it is characterised in that described flame-retarded resin is obtained by following steps:
1) epoxy resin is put in 100～150 DEG C of baking oven and preheat 7～9 hours, remove moisture and little volatile matters thing in resin
Matter；
2) weigh a small amount of liquid epoxies respectively to put in dough batch and mix in advance with quantitative firming agent, accelerator, fire retardant
Close, stir 20～40min, be respectively prepared firming agent and accelerator and flame retardant resin paste；
3) resin paste that step 2 is obtained is ground two to three times on three-roll grinder, obtains that viscosity is less, and powder diameter is more
Uniform firming agent and accelerator and flame retardant masterbatch；
4) epoxy resin of preheating is put into stirring in reactor, and froth in vacuum, cool to 80 DEG C simultaneously；
5) treat that resin temperature drops to 70～75 DEG C, be separately added into ground firming agent and accelerator and flame retardant masterbatch,
Mix 20～30 minutes in reactor high speed, powerful vacuum removes bubble removing simultaneously；
6) mixed resin is separately flowed into pallet under swager effect, by mono- piece of segmentation of 5kg, natural cooling at room temperature
Afterwards, pack by 6 pieces of a carton (30kg), obtain prepreg fire retarding epoxide resin system finished product.
5. method according to claim 3 is it is characterised in that described preimpregnation comprises the following steps:
1) draw fiber from creel, after regulation tension force, collection filament plate boundling, flattening process, reach the width of regulation；
2) draw ready made glued membrane from upper and lower glued membrane roller, and form sandwich structure with fiber, pass sequentially through several groups of hot pressing
Roller, makes resin matrix melt, in fiber embedded resin matrix；
3) cooling reduces prepreg temperature；
4) finally carry out trimming, cover pe film, winding, fire-retardant prepreg is obtained.
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| CN104387565A (en) * | 2014-11-17 | 2015-03-04 | 苏州苏月新材料有限公司 | Composite system of epoxy resin and curing agent for prepreg and preparation method of composite system |
| CN105000428B (en) * | 2015-07-15 | 2019-01-01 | 北京昂林贸烽科技有限公司 | A kind of equipment and its process for expansion fiber beam |
| CN105150404B (en) * | 2015-07-15 | 2018-06-19 | 北京昂林贸烽科技有限公司 | A kind of carbon fibre tow processing and treating method |
| CN105367997A (en) * | 2015-11-20 | 2016-03-02 | 国网浙江省电力公司台州供电公司 | Carbon fiber reinforcement phase epoxy resin based reinforced flame retardant composite material |
| CN107084035A (en) * | 2016-11-05 | 2017-08-22 | 芜湖市元山机械制造有限公司 | A kind of heavy-duty car silencing exhaust pipe high-termal conductivity packing material |
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| CN109664435A (en) * | 2018-06-07 | 2019-04-23 | 中山市富达运动器材有限公司 | A kind of manufacture craft of fibre knitting cloth |
| CN109159473A (en) * | 2018-10-25 | 2019-01-08 | 沈逸 | A kind of production method of sofa Packaging Box |
| CN109666297B (en) * | 2018-11-30 | 2021-08-03 | 中国航空工业集团公司基础技术研究院 | Ultraviolet fluorescent bismaleimide resin carbon fiber prepreg for sacrificial layer |
| CN112677581B (en) * | 2020-12-28 | 2023-11-14 | 芜湖小天鹅制冷设备有限公司 | Carbon fiber prepreg and preparation method and application thereof |
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