CN109929219A - Modified flame-retardant epoxy resin, prepreg and respective preparation method - Google Patents
Modified flame-retardant epoxy resin, prepreg and respective preparation method Download PDFInfo
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- CN109929219A CN109929219A CN201711378103.1A CN201711378103A CN109929219A CN 109929219 A CN109929219 A CN 109929219A CN 201711378103 A CN201711378103 A CN 201711378103A CN 109929219 A CN109929219 A CN 109929219A
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Abstract
The present invention provides modified flame-retardant epoxy resin, prepreg and respective preparation method, the method for preparing modified flame-retardant epoxy resin includes: to mix aminated carbon nano tube, fire retardant and epoxy resin, forms epoxy resin composition；Epoxy resin composition and curing agent are blended, modified flame-retardant epoxy resin is obtained.Aminated carbon nano tube is grafted in epoxy molecule chain, while improving the flame retardant property and mechanical property of material by the present invention by addition fire retardant and amination modified carbon nanotube.
Description
Technical field
The present invention relates to Material Fields, more particularly, to modified flame-retardant epoxy resin, prepreg and respective preparation side
Method.
Background technique
Common resin system has phenolic resin, epoxy resin, bismaleimide resin and cyanate ester resin in advanced composite material
Deng wherein epoxy resin has excellent adhesion energy, wear-resisting property, electrical insulation capability, chemical stability.Prepreg is multiple
The intermediate materials of condensation material preparation process, the superiority and inferiority of quality directly influence the quality of final product composite material.However ring
Oxygen resin has the characteristics that be easy burning, and based on environmental requirement, the current method for improving epoxy group prepreg flame retardant property is to add
Add phosphorus nitrogen reactive flame retardant to improve the anti-flammability of epoxy resin, however the above method is the anti-flammability for paying close attention to material
Can, the comprehensive performance for improving material is not considered how, for example, mechanical property, to limit answering for flame retardant composite material
Use range.
Summary of the invention
The present invention provides a kind of epoxy resin-matrix prepregs, pass through addition halogen-free environment-friendlyflame flame retardant and modified carbon nano tube
Pipe, while the fire-retardant and mechanical property of material is improved, it overcomes epoxy resin and is easy burning, mechanical property (especially impact
Can) difference disadvantage.
The present invention provides a kind of methods for preparing modified flame-retardant epoxy resin, comprising: by aminated carbon nano tube, fire-retardant
Agent and epoxy resin mixing, form epoxy resin composition；The epoxy resin composition and curing agent are blended, obtained
The modified flame-retardant epoxy resin.
In the above-mentioned methods, in the epoxy resin composition, the aminated carbon nano tube, the fire retardant and institute
Stating the ratio between parts by weight of epoxy resin is 80:10-15:5-10.
In the above-mentioned methods, the ratio between parts by weight of the epoxy resin composition and the curing agent are 5-8:1-4.
In the above-mentioned methods, the curing agent includes one of polyamide, m-phenylene diamine (MPD) and benzene dimethylamine or more
Kind.
In the above-mentioned methods, the aminated carbon nano tube is prepared by following steps: carbon nanotube is added to dense sulphur
Acid is reacted with nitric acid, is centrifuged, and is washed, freeze-drying, obtains acidification carbon nanotube；By the acidification carbon nanotube and second two
Amine and catalyst are reacted, and the aminated carbon nano tube is obtained after centrifugal drying.
In the above-mentioned methods, the ratio between parts by weight of the carbon nanotube, the ethylenediamine and the catalyst are 10:
10-15:2-5。
The present invention also provides the modified flame-retardant epoxy resin prepared by the above method.
The present invention also provides a kind of methods for preparing prepreg, comprising: is coated on above-mentioned modified flame-retardant epoxy resin
It in fiber cloth, is impregnated with, squeezes, winding obtains the prepreg.
In the above-mentioned methods, temperature when being coated with the modified flame-retardant epoxy resin is 70 DEG C -80 DEG C, the temperature of the impregnation
Degree is 90 DEG C -100 DEG C.
The present invention also provides the prepregs prepared by the above method.
Aminated carbon nano tube is grafted to asphalt mixtures modified by epoxy resin by addition fire retardant and amination modified carbon nanotube by the present invention
In rouge strand, while improving the flame retardant property and mechanical property of modified epoxy and prepreg.
Detailed description of the invention
Fig. 1 shows the schematic diagram of glue film preparation.
Fig. 2 shows the schematic diagrames of prepreg preparation.
Specific embodiment
Aminated carbon nano tube is grafted to asphalt mixtures modified by epoxy resin by addition fire retardant and amination modified carbon nanotube by the present invention
In rouge strand, while improving the flame retardant property and mechanical property of composite material.
The preparation process of aminated carbon nano tube is described below.Under conditions of ice bath, 10 parts of carbon nanotubes are added to
In 14~16 parts of concentrated sulfuric acids and 11~13 parts of nitric acid, it is then warming up to 70~90 DEG C of 10~14h of reaction.By obtained solution into
Obtained black solid is freeze-dried, is acidified with ethyl alcohol, hydrochloric acid and after distilling water washing three times by row centrifugation
Carbon nanotube.Acidification carbon nanotube is placed in a beaker afterwards, 10~15 parts of ethylenediamines and 2~5 parts of 2- (7- oxidation benzos are added
Triazole)-N, N, N', N'- tetramethylurea hexafluorophosphoric acid ester (HATU) 10~14h of catalyst reaction obtains ammonia after centrifugal drying
Base carbon nano tube.Unless otherwise indicated, number of the invention is parts by weight.
Later, aminated carbon nano tube, fire retardant and epoxy resin are mixed, forms epoxy resin composition.Wherein, may be used
It is mixed, is conducive in this way by amination with epoxy resin with adding organic solvent (for example, ethyl alcohol) for aminated carbon nano tube
Carbon nanotube spreads more evenly across in the epoxy.Then by epoxy resin composition by way of mechanical stirring and ultrasound
It is blended with curing agent, obtains modified flame-retardant epoxy resin.The wherein ratio of each component are as follows: epoxy resin composition 50-80
Part, 10-40 parts of curing agent.In epoxy resin composition include 80 parts of epoxy resin, 10-15 parts of fire retardant, amination carbon nanometer
5-10 parts of pipe.Curing agent may include one of polyamide, m-phenylene diamine (MPD) and benzene dimethylamine or a variety of.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator, after carrying out glue film processing as shown in Figure 1
It is impregnated with containing dipping machine, after Extruded roller extrusion process, removes the modified flame-retardant asphalt mixtures modified by epoxy resin of high strength fibre cloth surface residual
Rouge, film temperature are 70 DEG C -80 DEG C, and impregnation temperature is 95 DEG C, finally wind, obtain fiber cloth/modified flame-retardant epoxy resin prepolymer
Leaching material.Fig. 1 shows the schematic diagram of glue film preparation.Wherein 1 is film collecting roller, and 2 be coating head and 3 be release paper bowl.Fig. 2 shows
The schematic diagram of prepreg preparation is gone out.Wherein, 4 be glue film roller, and 5 be prepreg wind-up roll, and 6 be overlay film roller, and 7 be heating plate.
Prepreg is subjected to laying, in 100~120 DEG C of vacuum drying oven heating, 0.5~1.5h, 140~160 DEG C of solidifications 1~
3h obtains fiber cloth/modified flame-retardant epoxy resin composite material.
Aminated carbon nano tube is added in epoxy resin as nanofiller, with curing reaction, amination nanotube
It is covalently attached with epoxy resin, with the increase of additive amount, the mechanical property of epoxy resin is improved, and aminated carbon nano tube
It is used as barrier in the epoxy, is capable of the propagation of trap heat and the entrance of oxygen, can be reduced in a small amount of addition fire-retardant
The additive amount of agent improves the flame retardant property of material；And additive amount it is excessive when expanding fire retardant phosphate can be hindered to play a role, and
Phosphate is reduced with respect to additive amount, declines the flame retardant property of epoxy resin.Fire retardant of the invention selects phosphate, but this is only
It is example, the invention is not limited thereto.
It is illustrated below with reference to specific embodiment, to better understand the invention.
Embodiment 1
10 parts of carbon nanotubes are added in 15 parts of concentrated sulfuric acids and 12 parts of nitric acid, 80 DEG C of reaction 12h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 13 parts of ethylenediamines and 3 parts of catalyst are added
HATU reacts 12h, obtains aminated carbon nano tube after centrifugal drying.
5 parts of aminated carbon nano tubes, 8 parts of phosphates and 50 parts of epoxy resin are mixed, form epoxy resin composition, so
Epoxy resin composition and 20 parts of polyamides are blended by way of mechanical stirring and ultrasound afterwards, obtain modified resistance
Fire epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual, wherein film temperature is after Extruded roller extrusion process
70 DEG C, impregnation temperature is 90 DEG C, finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Embodiment 2
10 parts of carbon nanotubes are added in 14 parts of concentrated sulfuric acids and 11 parts of nitric acid, 70 DEG C of reaction 10h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 10 parts of ethylenediamines and 5 parts of catalyst are added
HATU reacts 10h, obtains aminated carbon nano tube after centrifugal drying.
2.5 parts of aminated carbon nano tubes, 5 parts of phosphates and 40 parts of epoxy resin are mixed, epoxy resin composition is formed,
Then epoxy resin composition and 8 parts of m-phenylene diamine (MPD)s are blended by way of mechanical stirring and ultrasound, obtain modified resistance
Fire epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual after Extruded roller extrusion process, and film temperature is 80 DEG C,
Being impregnated with temperature is 100 DEG C, finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Embodiment 3
10 parts of carbon nanotubes are added in 16 parts of concentrated sulfuric acids and 13 parts of nitric acid, 90 DEG C of reaction 14h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 15 parts of ethylenediamines and 5 parts of catalyst are added
HATU reacts 14h, obtains aminated carbon nano tube after centrifugal drying.
8 parts of aminated carbon nano tubes, 12 parts of phosphates and 64 parts of epoxy resin are mixed, epoxy resin composition is formed,
Then epoxy resin composition and 32 parts of benzene dimethylamines are blended by way of mechanical stirring and ultrasound, obtain modified resistance
Fire epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual after Extruded roller extrusion process, and film temperature is 72 DEG C,
Being impregnated with temperature is 92 DEG C, it finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Embodiment 4
10 parts of carbon nanotubes are added in 16 parts of concentrated sulfuric acids and 12 parts of nitric acid, 80 DEG C of reaction 12h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 13 parts of ethylenediamines and 2 parts of catalyst are added
HATU reacts 12h, obtains aminated carbon nano tube after centrifugal drying.
5 parts of aminated carbon nano tubes, 8 parts of phosphates and 50 parts of epoxy resin are mixed, form epoxy resin composition, so
Epoxy resin composition and 20 parts of polyamides are blended by way of mechanical stirring and ultrasound afterwards, obtain modified resistance
Fire epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual after Extruded roller extrusion process, and film temperature is 75 DEG C,
Being impregnated with temperature is 95 DEG C, finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Embodiment 5
10 parts of carbon nanotubes are added in 15 parts of concentrated sulfuric acids and 12 parts of nitric acid, 80 DEG C of reaction 12h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 14 parts of ethylenediamines and 3 parts of catalyst are added
HATU reacts 12h, obtains aminated carbon nano tube after centrifugal drying.
6 parts of aminated carbon nano tubes, 8 parts of phosphates and 50 parts of epoxy resin are mixed, form epoxy resin composition, so
Epoxy resin composition and 20 parts of m-phenylene diamine (MPD)s are blended by way of mechanical stirring and ultrasound afterwards, obtain modified flame-retardant
Epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual after Extruded roller extrusion process, and film temperature is 78 DEG C,
Being impregnated with temperature is 98 DEG C, finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Embodiment 6
10 parts of carbon nanotubes are added in 15 parts of concentrated sulfuric acids and 12 parts of nitric acid, 80 DEG C of reaction 12h are then warming up to.By institute
Obtained solution is centrifuged, and after ethyl alcohol, hydrochloric acid and distillation water washing, obtained black solid is freeze-dried,
Obtain acidification carbon nanotube.Obtained acidification carbon nanotube is placed in a beaker, 12 parts of ethylenediamines and 3 parts of catalyst are added
HATU reacts 12h, obtains aminated carbon nano tube after centrifugal drying.
5 parts of aminated carbon nano tubes, 8 parts of phosphates and 50 parts of epoxy resin are mixed, form epoxy resin composition, so
Epoxy resin composition and 20 parts of benzene dimethylamines are blended by way of mechanical stirring and ultrasound afterwards, obtain modified flame-retardant
Epoxy resin.
The modified flame-retardant epoxy resin of above-mentioned preparation is subjected to film with film applicator in fiber cloth, is contained with containing dipping machine
Leaching removes the modified flame-retardant epoxy resin of fiber cloth surface residual after Extruded roller extrusion process, and film temperature is 75 DEG C,
Being impregnated with temperature is 95 DEG C, finally winds, obtains fiber cloth/modified flame-retardant epoxy prepreg.
Later, according to testing standard ASTM D638,695 ASTMD, ASTMD 3486 and GB/T3355-2005 to modification
Fire retarding epoxide resin and prepreg are processed, and test its related mechanical property.It is carried out according to testing standard as defined in UL-94
Flame retardant property test.It is of course also possible to use other suitable test methods.The structure of test is as shown in table 1.Modified flame-retardant ring
The bending strength of oxygen resin and the raising percentage of impact strength are for being not added with aminated carbon nano tube.Preimpregnation
The layer shear strength of material and the raising percentage of impact strength are also relative to the preimpregnation for being not added with aminated carbon nano tube formation
For material.
Table 1
From the foregoing, it will be observed that the modified flame-retardant epoxy resin prepared through the invention, vertical combustion grade can reach V-0 grades,
Relative to the epoxy resin for being not added with aminated carbon nano tube, bending strength improves 30% or more, and impact strength improves 20%
More than.The layer shear strength of the prepreg formed by modified flame-retardant epoxy resin improves 15% or more, and impact strength improves 10%
More than.That is, modified flame-retardant epoxy resin and prepreg of the invention is while keeping preferable flame retardant property, mechanical property
Significant raising is obtained.
Aminated carbon nano tube is grafted to asphalt mixtures modified by epoxy resin by addition fire retardant and amination modified carbon nanotube by the present invention
In rouge strand, while the flame retardant property and mechanical property of composite material are improved, solving fire retardant addition leads to prepreg
The problem of mechanical properties decrease.
Modified flame-retardant epoxy resin prepared by the present invention has excellent mechanical property, and flame retardant property, prepared answers
Condensation material can be applied to radome, space shuttle wing, space flight heat-barrier material, fuselage civil aircraft internal material, warship
The numerous areas such as ship surfacing and construction timber.
Claims (10)
1. a kind of method for preparing modified flame-retardant epoxy resin characterized by comprising
Aminated carbon nano tube, fire retardant and epoxy resin are mixed, epoxy resin composition is formed；
The epoxy resin composition and curing agent are blended, the modified flame-retardant epoxy resin is obtained.
2. the method according to claim 1, wherein in the epoxy resin composition, the amination carbon
The ratio between parts by weight of nanotube, the fire retardant and the epoxy resin are 80:10-15:5-10.
3. the method according to claim 1, wherein the weight of the epoxy resin composition and the curing agent
The ratio between number is 5-8:1-4.
4. the method according to claim 1, wherein the curing agent include polyamide, m-phenylene diamine (MPD) and
One of benzene dimethylamine is a variety of.
5. the method according to claim 1, wherein preparing the aminated carbon nano tube by following steps:
Carbon nanotube is added in the concentrated sulfuric acid and nitric acid, is reacted, is centrifuged, is washed, freeze-drying obtains acidification carbon nanotube；
The acidification carbon nanotube is reacted with ethylenediamine and catalyst, the amination carbon nanometer is obtained after centrifugal drying
Pipe.
6. according to the method described in claim 5, it is characterized in that, the carbon nanotube, the ethylenediamine and the catalyst
The ratio between parts by weight be 10:10-15:2-5.
7. the modified flame-retardant epoxy resin of method preparation according to any one of claim 1 to 6.
8. a kind of method for preparing prepreg characterized by comprising
Modified flame-retardant epoxy resin according to claim 7 is coated in fiber cloth, is impregnated with, is squeezed, winding obtains institute
State prepreg.
9. according to claim 8 in method, which is characterized in that temperature when being coated with the modified flame-retardant epoxy resin is 70
DEG C -80 DEG C, the temperature of the impregnation is 90 DEG C -100 DEG C.
10. according to the prepreg of the described in any item method preparations of claim 8-9.
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| CN105778424A (en) * | 2016-04-22 | 2016-07-20 | 武汉理工大学 | Carbon nanotube and carbon fiber synergistically modified epoxy resin composite material and preparation method thereof |
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2017
- 2017-12-19 CN CN201711378103.1A patent/CN109929219A/en active Pending
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| CN101104726A (en) * | 2006-07-14 | 2008-01-16 | 同济大学 | Preparation method for carbon nano-tube/epoxy resin high-performance composite material |
| CN102250447A (en) * | 2010-05-21 | 2011-11-23 | 台燿科技股份有限公司 | Halogen-free fire resistance epoxy resin composite as well as prepreg material and printed circuit board therefrom |
| CN105778424A (en) * | 2016-04-22 | 2016-07-20 | 武汉理工大学 | Carbon nanotube and carbon fiber synergistically modified epoxy resin composite material and preparation method thereof |
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