CN104002523A - 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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- CN104002523A CN104002523A CN201410157894.5A CN201410157894A CN104002523A CN 104002523 A CN104002523 A CN 104002523A CN 201410157894 A CN201410157894 A CN 201410157894A CN 104002523 A CN104002523 A CN 104002523A
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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, particularly relate to a kind of carbon fiber prepreg with flame retardant effect.
Background technology
Carbon fiber is the indispensable strategic new material of national economy and national defense construction, it is one of most important reinforcement of advanced composite material, it has, and intensity is high, density is little, plasticity is strong, the advantages such as corrosion-resistant, the life-span is long, are therefore widely used in the fields such as Aero-Space, resource equipment, communications and transportation, architectural engineering, Leisure Sport.In prior art, carbon fiber prepreg is all the carbon fiber layers that are soaked with conventional epoxy resin, and because conventional epoxy resin does not have anti-flammability, therefore carbon fiber prepreg of the prior art can not be applied on electronics 3C Product.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of this invention is to provide and a kind ofly flood the carbon fiber prepreg that fire retarding epoxide resin has flame retardant effect, and the present invention also provides the preparation method of this carbon fiber prepreg.
To achieve these goals, the technical scheme that the present invention takes is as follows:
A fire-retardant carbon fiber prepreg, comprises carbon fiber layer and is immersed in fire retarding epoxide resin wherein, also comprises that direct note invests the release liners on carbon fiber layer outer surface.
Further, the fiber in described carbon fiber layer is that same direction parallel arranged group is established and formed, and utilizes fire retarding epoxide resin mutually to flood between carbon fiber.
A hot melt two step method preparation method for described carbon fiber prepreg, comprises masking and preimpregnation.
Further, described masking comprises the following steps:
1) flame-retarded resin matrix being placed in to blender fully mixes;
2) until rubber roll, be heated to after 70 ℃, be transported to glue spreader, regulate the spacing of glue spreader and the travel line speed of release liners, make the glued membrane of different-thickness;
3) with infrared ray instrument, detect the thickness of glued membrane or the surface density of glued membrane, by coldplate, reduce the temperature of glued membrane, reduce its state of cure;
4) rolling, packing, deposit in freezer stand-by.
Further, described flame-retarded resin is comprised of the component of following weight ratio:
ATN series of loops epoxy resins: 12-15%; E-51:15-20%; E-44:5-8%; E-20:40-45%; Micronizing dicyandiamide: 5-8%; Ureas promoter: 1-1.5%; Hydrated alumina: 10-15%; White carbon thickener: 0.5-1%.
Further, described flame-retarded resin makes by following steps:
1) epoxy resin is put into the baking oven preheating 7～9 hours of 100～150 ℃, removed moisture and little volatile matter material in resin;
2) weigh respectively a small amount of liquid epoxies and quantitative curing agent, promoter, fire retardant and put into dough batch and be pre-mixed, stir 20～40min, make respectively curing agent and promoter and fire retardant resin paste;
3) resin paste step 2 being made is ground two to three times on three-roll grinder, obtains viscosity less, and powder diameter is curing agent and promoter and fire retardant masterbatch more uniformly;
4) epoxy resin of preheating is put into reactor and stir, and froth in vacuum, cool to 80 ℃ simultaneously;
5) treat that resin temperature drops to 70～75 ℃, add respectively ground curing agent and promoter and fire retardant masterbatch, in reactor high speed, mix 20～30 minutes, powerful vacuum is removed bubble simultaneously;
6) mixed resin is flowed into respectively under swager effect to pallet, by mono-of 5kg, cuts apart, at room temperature naturally cooling after, by 6 (30kg) packings of a carton, obtain fire retarding epoxide resin system finished product for prepreg.
Further, described preimpregnation comprises the following steps:
1) from creel, draw fiber, after adjustment of tonicity, collection filament plate boundling, flattening program, reach the width of regulation;
2) from upper and lower glued membrane roller, draw ready made glued membrane, and form sandwich structure with fiber, successively by several groups of hot-pressing rollers, make resin matrix melting, in fiber embedded resin matrix;
3) cooling reduction prepreg temperature;
4) finally carry out trimming, cover PE film, rolling, make fire-retardant prepreg.
The present invention is not changing the flame retardant effect that has increased carbon fiber prepreg under current initial rinsing method prerequisite, overcome the carbon fiber prepreg of circulation in the market without flame retardant effect, can not use the problem at relevant special dimension, widened the range of application of carbon fiber product, the present invention simultaneously obtains carbon fiber prepreg by the mode of fire retarding epoxide resin preimpregnation carbon fiber, method is simple, and the product of production process and acquisition all meets environment-friendly products and requires (ROSH, Reach are all qualified).Carbon fiber prepreg of the present invention can be widely used in the 3C Product fields such as electronics, forms light weight, intensity is higher and has the carbon fiber product of flame retardant effect.
Accompanying drawing explanation
Fig. 1 is the flow chart of film making process of the present invention;
Fig. 2 is the flow chart of preimpregnation operation of the present invention.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Fire-retardant carbon fiber prepreg of the present invention, comprises carbon fiber layer and be immersed in fire retarding epoxide resin wherein, and directly note invests the release liners on carbon fiber layer outer surface.Fiber in described carbon fiber layer is that same direction parallel arranged group is established and formed, and utilizes fire retarding epoxide resin mutually to flood between carbon fiber.
Carbon fiber prepreg of the present invention is prepared by hot melt two step method, and this preparation method comprises masking and preimpregnation.Masking comprises step: 1) fire retarding epoxide resin matrix is placed in to blender and fully mixes; 2) until rubber roll, be heated to after 70 ℃, be transported to glue spreader, regulate the spacing of glue spreader and the travel line speed of release liners, make the glued membrane of different-thickness; 3) with infrared ray instrument, detect the thickness of glued membrane or the surface density of glued membrane, by coldplate, reduce the temperature of glued membrane, reduce its state of cure; 4) rolling, packing, deposit in freezer stand-by.Preimpregnation comprises step: 1) from creel, draw fiber, after adjustment of tonicity, collection filament plate boundling, flattening program, reach the width of regulation; 2) from upper and lower glued membrane roller, draw ready made glued membrane, and form sandwich structure with fiber, successively by several groups of hot-pressing rollers, make resin matrix melting, in fiber embedded resin matrix; 3) cooling reduction prepreg temperature; 4) finally carry out trimming, cover PE film, rolling, make fire-retardant prepreg.
Now by following examples, illustrate the preparation process of the fire retarding epoxide resin of the fire-retardant carbon fiber prepreg of the present invention.
embodiment 1
Described flame-retarded resin is comprised of the component of following weight ratio:
ATN series of loops epoxy resins: 12%; E-51:17%; E-44:6%; E-20:43%; Micronizing dicyandiamide: 5%; Ureas promoter: 1.5%; Hydrated alumina: 15%; White carbon thickener: 0.5%.
1) epoxy resin is put into the baking oven preheating 7 hours of 110 ℃, removed moisture and little volatile matter material in resin;
2) weigh respectively a small amount of liquid epoxies and quantitative curing agent, promoter, fire retardant and put into dough batch and be pre-mixed, stir 25min, make respectively curing agent and promoter and fire retardant resin paste;
3) resin paste step 2 being made is ground two to three times on three-roll grinder, obtains viscosity less, and powder diameter is curing agent and promoter and fire retardant masterbatch more uniformly;
4) epoxy resin of preheating is put into reactor and stir, and froth in vacuum, cool to 80 ℃ simultaneously;
5) treat that resin temperature drops to 70 ℃, add respectively ground curing agent and promoter and fire retardant masterbatch, in reactor high speed, mix 20 minutes, powerful vacuum is removed bubble simultaneously;
6) mixed resin is flowed into respectively under swager effect to pallet, by mono-of 5kg, cuts apart, at room temperature naturally cooling after, by 6 (30kg) packings of a carton, obtain fire retarding epoxide resin system finished product for prepreg.
embodiment 2
Described flame-retarded resin is comprised of the component of following weight ratio:
ATN series of loops epoxy resins: 13%; E-51:19%; E-44:5%; E-20:45%; Micronizing dicyandiamide: 6%; Ureas promoter: 1%; Hydrated alumina: 10%; White carbon thickener: 1%.
1) epoxy resin is put into the baking oven preheating 8 hours of 120 ℃, removed moisture and little volatile matter material in resin;
2) weigh respectively a small amount of liquid epoxies and quantitative curing agent, promoter, fire retardant and put into dough batch and be pre-mixed, stir 30min, make respectively curing agent and promoter and fire retardant resin paste;
3) resin paste step 2 being made is ground two to three times on three-roll grinder, obtains viscosity less, and powder diameter is curing agent and promoter and fire retardant masterbatch more uniformly;
4) epoxy resin of preheating is put into reactor and stir, and froth in vacuum, cool to 80 ℃ simultaneously;
5) treat that resin temperature drops to 75 ℃, add respectively ground curing agent and promoter and fire retardant masterbatch, in reactor high speed, mix 30 minutes, powerful vacuum is removed bubble simultaneously;
6) mixed resin is flowed into respectively under swager effect to pallet, by mono-of 5kg, cuts apart, at room temperature naturally cooling after, by 6 (30kg) packings of a carton, obtain fire retarding epoxide resin system finished product for prepreg.
embodiment 3
Described flame-retarded resin is comprised of the component of following weight ratio:
ATN series of loops epoxy resins: 15%; E-51:20%; E-44:5%; E-20:40%; Micronizing dicyandiamide: 8%; Ureas promoter: 1%; Hydrated alumina: 10%; White carbon thickener: 1%.
1) epoxy resin is put into the baking oven preheating 9 hours of 150 ℃, removed moisture and little volatile matter material in resin;
2) weigh respectively a small amount of liquid epoxies and quantitative curing agent, promoter, fire retardant and put into dough batch and be pre-mixed, stir 40min, make respectively curing agent and promoter and fire retardant resin paste;
3) resin paste step 2 being made is ground two to three times on three-roll grinder, obtains viscosity less, and powder diameter is curing agent and promoter and fire retardant masterbatch more uniformly;
4) epoxy resin of preheating is put into reactor and stir, and froth in vacuum, cool to 80 ℃ simultaneously;
5) treat that resin temperature drops to 73 ℃, add respectively ground curing agent and promoter and fire retardant masterbatch, in reactor high speed, mix 25 minutes, powerful vacuum is removed bubble simultaneously;
6) mixed resin is flowed into respectively under swager effect to pallet, by mono-of 5kg, cuts apart, at room temperature naturally cooling after, by 6 (30kg) packings of a carton, obtain fire retarding epoxide resin system finished product for prepreg.
The resin that above embodiment is obtained carries out anti-flammability test, and testing equipment is: level-testing vertical flammability instrument, model: RH-6033B; Probe temperature: 22.5 ℃, humidity: 51%RH; Normative reference: the flammability test of plastic material for UL94-2013 equipment and device component; Testing process: instrument parameter → test is set; Sample size: 130mm * 13mm * 1mm; Sample pretreatment: at 23 ± 2 ℃, 50 ± 5%RH environmental condition is placed 48h.
Testing procedure: flame height 20 ± 1mm, Bunsen burner is placed in sample below center position, the Bunsen burner mouth of pipe is apart from sample bottom 10 ± 1mm, be 10 ± 0.5s the duration of ignition, after igniting 10 ± 0.5s, with the speed of 300mm/sec, remove at least 150mm of Bunsen burner, start to record residual flame time t1 simultaneously, when residual flame stops, should lighting immediately 10 ± 0.5s, after igniting 10 ± 0.5s, with the speed of 300mm/sec, remove at least 150mm of Bunsen burner, record residual flame time t2 and Yu Ran time t3 simultaneously.
Judgment criteria:
According to above step and judgment criteria, the product making from described three embodiment, to choose arbitrarily 5 and test and compare with conventional resin, test result is as follows:
By relatively can finding out of above test result, fire retarding epoxide resin used in the present invention meets the fire-retardant requirement of UL94-V1.
More than describe the preferred embodiments of the present invention in detail, but the present invention is not limited to these embodiment, in application range of the present invention, can carries out various changes.Although just elaborated the preferred embodiments of the present invention above,, person of ordinary skill in the field is very clear substantially not to be departed from the scope of novelty of the present invention and advantage, can carry out various modifications to exemplary embodiment.
Claims (7)
1. a fire-retardant carbon fiber prepreg, is characterized in that, comprises carbon fiber layer and fire retarding epoxide resin, and wherein fire retarding epoxide resin is immersed in carbon fiber layer; And directly note invests the release liners on carbon fiber layer outer surface.
2. fire-retardant carbon fiber prepreg according to claim 1, is characterized in that, the fiber in described carbon fiber layer is that same direction parallel arranged group is established and formed, and utilizes fire retarding epoxide resin mutually to flood between carbon fiber.
3. a hot melt two step method preparation method for carbon fiber prepreg claimed in claim 1, is characterized in that, comprises masking and preimpregnation.
4. preparation method according to claim 3, is characterized in that, described masking comprises the following steps:
1) flame-retarded resin matrix being placed in to blender fully mixes;
2) until rubber roll, be heated to after 70 ℃, be transported to glue spreader, regulate the spacing of glue spreader and the travel line speed of release liners, make the glued membrane of different-thickness;
3) with infrared ray instrument, detect the thickness of glued membrane or the surface density of glued membrane, by coldplate, reduce the temperature of glued membrane, reduce its state of cure;
4) rolling, packing, deposit in freezer stand-by.
5. method according to claim 4, is characterized in that, described flame-retarded resin is comprised of the component of following weight ratio:
ATN series of loops epoxy resins: 12～15%; E-51:15～20%; E-44:5～8%; E-20:40～45%; Micronizing dicyandiamide: 5～8%; Ureas promoter: 1～1.5%; Hydrated alumina: 10～15%; White carbon thickener: 0.5～1%.
6. method according to claim 4, is characterized in that, described flame-retarded resin makes by following steps:
1) epoxy resin is put into the baking oven preheating 7～9 hours of 100～150 ℃, removed moisture and little volatile matter material in resin;
2) weigh respectively a small amount of liquid epoxies and quantitative curing agent, promoter, fire retardant and put into dough batch and be pre-mixed, stir 20～40min, make respectively curing agent and promoter and fire retardant resin paste;
3) resin paste step 2 being made is ground two to three times on three-roll grinder, obtains viscosity less, and powder diameter is curing agent and promoter and fire retardant masterbatch more uniformly;
4) epoxy resin of preheating is put into reactor and stir, and froth in vacuum, cool to 80 ℃ simultaneously;
5) treat that resin temperature drops to 70～75 ℃, add respectively ground curing agent and promoter and fire retardant masterbatch, in reactor high speed, mix 20～30 minutes, powerful vacuum is removed bubble simultaneously;
6) mixed resin is flowed into respectively under swager effect to pallet, by mono-of 5kg, cuts apart, at room temperature naturally cooling after, by 6 (30kg) packings of a carton, obtain fire retarding epoxide resin system finished product for prepreg.
7. method according to claim 3, is characterized in that, described preimpregnation comprises the following steps:
1) from creel, draw fiber, after adjustment of tonicity, collection filament plate boundling, flattening program, reach the width of regulation;
2) from upper and lower glued membrane roller, draw ready made glued membrane, and form sandwich structure with fiber, successively by several groups of hot-pressing rollers, make resin matrix melting, in fiber embedded resin matrix;
3) cooling reduction prepreg temperature;
4) finally carry out trimming, cover PE film, rolling, make fire-retardant prepreg.
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Cited By (11)
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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 |
| CN105000428A (en) * | 2015-07-15 | 2015-10-28 | 北京昂林贸烽科技有限公司 | Equipment and technological method for expansion of fiber bundles |
| CN105150404A (en) * | 2015-07-15 | 2015-12-16 | 北京昂林贸烽科技有限公司 | Method for processing carbon fiber tow |
| 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 |
| CN108556110A (en) * | 2018-04-24 | 2018-09-21 | 浙江省林业科学研究院 | A kind of manufacturing method of bamboo beam veneer LCM formed fitment components |
| CN108943772A (en) * | 2017-12-14 | 2018-12-07 | 中航复合材料有限责任公司 | A kind of fast preparation method of high-performance composite materials sheet material |
| CN109159473A (en) * | 2018-10-25 | 2019-01-08 | 沈逸 | A kind of production method of sofa Packaging Box |
| CN109666297A (en) * | 2018-11-30 | 2019-04-23 | 中国航空工业集团公司基础技术研究院 | A kind of sacrificial layer Ultraluminescence bimaleimide resin carbon fiber prepreg |
| 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 |
| CN112677581A (en) * | 2020-12-28 | 2021-04-20 | 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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Cited By (14)
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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 |
| CN105000428A (en) * | 2015-07-15 | 2015-10-28 | 北京昂林贸烽科技有限公司 | Equipment and technological method for expansion of fiber bundles |
| CN105150404A (en) * | 2015-07-15 | 2015-12-16 | 北京昂林贸烽科技有限公司 | Method for processing carbon fiber tow |
| 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 |
| CN108943772A (en) * | 2017-12-14 | 2018-12-07 | 中航复合材料有限责任公司 | A kind of fast preparation method of high-performance composite materials sheet material |
| CN108556110A (en) * | 2018-04-24 | 2018-09-21 | 浙江省林业科学研究院 | A kind of manufacturing method of bamboo beam veneer LCM formed fitment components |
| CN108556110B (en) * | 2018-04-24 | 2023-04-11 | 浙江省林业科学研究院 | Manufacturing method of bamboo bundle veneer LCM (liquid Crystal Module) molded furniture component |
| 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 |
| CN109666297A (en) * | 2018-11-30 | 2019-04-23 | 中国航空工业集团公司基础技术研究院 | A kind of sacrificial layer Ultraluminescence bimaleimide resin carbon fiber prepreg |
| 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 |
| CN112677581A (en) * | 2020-12-28 | 2021-04-20 | 芜湖小天鹅制冷设备有限公司 | Carbon fiber prepreg and preparation method and application thereof |
| 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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