CN105968717B - A kind of preparation of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg and carbon fibre composite - Google Patents
A kind of preparation of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg and carbon fibre composite Download PDFInfo
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- CN105968717B CN105968717B CN201610339807.7A CN201610339807A CN105968717B CN 105968717 B CN105968717 B CN 105968717B CN 201610339807 A CN201610339807 A CN 201610339807A CN 105968717 B CN105968717 B CN 105968717B
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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
- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2409/02—Copolymers with acrylonitrile
Abstract
A kind of preparation of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg and carbon fibre composite, belong to field of composite material preparation, the present invention carries out chemical modification by graphene, and binary reinforcer is formed with multi-walled carbon nanotube, is advantageous to reinforcement in the base scattered；The combination matrix of epoxy resin liquid XNBR is provided, the present invention is prepared for continuous carbon fibre composite material using the compound of material of more sizes, improves the mechanical property of composite.When graphene/carbon nano-tube content reaches 1.0wt%, interlaminar shear strength reaches 87.90MPa, and when graphene/carbon nano-tube content reaches 2.0wt%, tensile strength reaches maximum 64.31MPa.
Description
Technical field
The present invention relates to the system of a kind of carbon fiber/graphite alkene/carbon nano tube/epoxy resin leaching material and carbon fibre composite
A kind of Preparation Method, and in particular to method that composite is prepared using rubber-composition epoxy resin as matrix.
Background technology
Modern development in science and technology is rapid, and application of the composite in terms of Aero-Space is also increasingly wider, while people are to multiple
The requirement of the performance of condensation material is also more and more harsh.Being dispersed into for composite material reinforcement body and basal body interface and reinforcement is multiple
The bottleneck of condensation material performance boost, the physics of composite material reinforcement body and chemical micro-structural are changed based on across scale Design thought,
Solve interface problem and scattering problem simultaneously turns into an important research direction to improve the mechanical property of composite.
Carbon material such as graphene, CNT etc. have excellent mechanical property, are usually utilized to as reinforcement, but
The hydrophobicity of grapheme material limits its use, and by chemical modification, introducing polar group can have on graphene sheet layer
The hydrophily of effect increase grapheme material, while suppress its reunion.Carbon material is divided into the fullerene of zero dimension, one-dimensional CNT
, can be in resin matrix by the synergy of the carbon material of both or three kinds of different dimensions with the grapheme material of two dimension
Network structure is formed, more efficiently transmits load, lifts mechanical property.
Carbon fiber epoxy based composites are the very extensive composites of a kind of research, are introduced in resin matrix
Thermoplastic rubber material can effectively improve the fragility increase toughness of epoxy resin, while add modified graphene/carbon nanometer
Pipe is dispersed in epoxy resin-rubber composition as reinforcement.Different scale reinforcement synergy, in difference
Dimension play and transmit the effect of load and can effectively lift the mechanical properties of carbon fiber epoxy based composites.
The content of the invention
In order to obtain the more excellent carbon fiber enhancement resin base composite material of performance, the invention provides one kind to prepare carbon
The preparation method of fiber/graphene/carbon nano-tube/epoxy prepreg and carbon fibre composite
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg, comprises the following steps successively：
Step 1：Prepare graphene
It is preferred that use following methods：
Weigh NaNO3Solid is dissolved in 98% concentrated sulfuric acid, is placed in ice-water bath and is added rotor and is stirred continuously, and adds scale
Graphite, 30min is persistently stirred, be slowly added to KMnO4, kept for 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；
Add deionized water (being such as slowly added in 10min) and then heat to 98 DEG C, 15min is kept in the temperature；Add pre- in advance
Heat adds hydrogen peroxide, terminating reaction, and stir 10min until no longer producing bubble to 50 DEG C of deionized water；Configuration about 5%
Hydrochloric acid solution, be added in reaction solution, centrifugation precipitated；Washed repeatedly with deionized water and be precipitated to centrifugate pH=7,
Graphene oxide is obtained by gained precipitation is lyophilized, takes gained graphene oxide, is quickly put into and is preheated to 1050 DEG C of Muffle furnace
Middle holding several seconds expanded graphite alkene；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h or so, obtains stone
Black alkene；
Step 2：Graphene is dissolved in dimethylformamide and forms the equal of 0.1-1mg/mL (preferably 0.33mg/mL)
Even dispersion liquid, the dimethyl formamide solution of isocyanates is added dropwise into above-mentioned graphene dispersing solution and continues to stir, mixing is molten
Liquid in a nitrogen atmosphere, 75-85 DEG C of reaction 0.5-1.5h (preferably 80 DEG C reaction 1h), then washs precipitation with dimethylformamide
Several times, the dimethyl formamide solution of MDA is added into precipitation and continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally
By centrifugation, dimethylformamide washing, vacuum drying obtains modified graphene；
Step 3：Prepare epoxy resin (such as E-51), curing agent MeTHPA and liquid XNBR mass ratio are
100:60-80:8-12 (preferably 100:70:11) resin-rubbery system and epoxy resin (such as E-51), curing agent diaminourea two
The mass ratio of phenylmethane (DDM) and liquid XNBR is 100:30-40:8-12 (preferably 100:35:11) resin-rubber
Colloid system, then add multi-walled carbon nanotube and modified graphene, the addition quality phase of multi-walled carbon nanotube and modified graphene
Deng weight/mass percentage composition is 0.05wt%-1.0wt%；Then, after mechanical agitation and ultrasonic reaction 5-7h, accelerator is added
2,4,6- tri- (dimethylamino methyl) phenol (DMP-30), and continue ultrasonic reaction (such as one hour or so) for a period of time；Then,
Place reaction liquid into and be preheated to de-bubbled at least 0.5h in 50 DEG C of vacuum drying oven, obtain modified graphene/CNT/epoxy
Resin slurry；
Step 4：Modified graphene/carbon nano tube/epoxy resin slurry is poured into steeping vat, and put in steeping vat
Supersonic generator is put, carbon fiber is immersed in modified graphene/carbon nano tube/epoxy resin slurry, control operating power exists
120-170W；It is 8-15s to control the impregnation time, and tow tension is 160-200 grams, is removed after the completion of impregnation by a spreading roller
Unnecessary resin adhesive liquid；
Step 5：Tow after impregnation arranges silk by way of arranging silk machine using winding, is wound, preferably amounted to repeatedly
3-5 layers are wound repeatedly, form unidirectional prepreg cloth；
Step 6：Prepreg cloth is removed, 7-12h is dried under 50-70 DEG C of vacuum condition；Then dried at 100-120 DEG C
4-6h, obtain carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg；
In above-mentioned steps two, graphene：Isocyanates：MDA uses magnitude relation 100mg：0.005-0.1mol：0.05-
0.1mol。
Carbon fibre composite, it is characterised in that carbon fiber/graphite alkene/CNT/resin prepreg material is passed through into hot pressing
Machine prepares laminate (if pressure used is 5MPa), and temperature-rise period is：90 DEG C, 1h；130 DEG C, 2h；150 DEG C, 2h, Ran Houbao
Pressure is cooled to room temperature and obtains carbon fiber/graphite alkene/carbon nano tube/epoxy resin composite material.
One-dimensional CNT can improve the stacking of graphene, on the one hand so enable to filler to disperse in the base equal
It is even so that filler forms a good bridge linking effect between matrix and carbon fiber；On the other hand, graphene and carbon nanometer
The conductive mesh structure formed between pipe, is more beneficial for the raising of composite heat endurance.Answered compared to traditional carbon fiber
Condensation material, the presence of the Nano filling of two kinds of dimensions, the cooperative effect between filler is not only played, it is often more important that two kinds are filled out
Dimensionality effect between material be present, be advantageous to improve the mechanical property of composite.
Compared with immediate prior art, technical scheme provided by the invention has following excellent effect：
When it is 0.5wt% that modified graphene and CNT, which respectively account for epoxy-resin systems content, carbon fiber/graphite
The tensile strength of alkene/CNT reinforced epoxy base unidirectional composite material respectively reaches 60.02MPa with interlaminar shear strength
And 87.80MPa, 14.1% He has been respectively increased compared to the carbon-fibre reinforced epoxy resin composite material for being not added with any filler
10.1%.When it is 1.0wt% that modified graphene and CNT, which respectively account for epoxy-resin systems content, carbon fiber/graphite alkene/
The tensile strength of CNT reinforced epoxy base unidirectional composite material and interlaminar shear strength respectively reach 63.53MPa and
82.17MPa, 20.7% He is respectively increased compared to the carbon-fibre reinforced epoxy resin composite material for being not added with any filler
3.0%.
Embodiment
Below by embodiment, the present invention is described in further detail, but the present invention is not limited to following examples.
Embodiment 1
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
Under gas atmosphere, 80 DEG C of temperature reaction 1h, then wash precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
The mass ratio for preparing epoxy resin (E-51), curing agent (MeTHPA) and liquid XNBR is 100:70:
11 resin-rubber solutions, the multi-walled carbon nanotube that equal proportion adds 0.1wt% (0.05wt% respectively) arrive with modified graphene
In resin system solution.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator (DMP-30) is added, and continue to surpass
Phonoresponse 1h.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven, obtain resin-rubber slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Embodiment 2
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
80 DEG C of temperature reaction 1h under gas atmosphere, then washs precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
The mass ratio for preparing epoxy resin (E-51), curing agent (MeTHPA) and liquid XNBR is 100:70:
11 resin-rubber solutions, the multi-walled carbon nanotube that equal proportion adds 0.5wt% (0.25wt% respectively) arrive with modified graphene
In resin system solution.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator (DMP-30) is added, and continue to surpass
Phonoresponse 1h.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven, obtain resin-rubber slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Embodiment 3
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
80 DEG C of temperature reaction 1h under gas atmosphere, then washs precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
The mass ratio for preparing epoxy resin (E-51), curing agent (MeTHPA) and liquid XNBR is 100:70:
11 resin-rubber solutions, the multi-walled carbon nanotube that equal proportion adds 1.0wt% (0.5wt% respectively) arrive with modified graphene
In resin system solution.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator (DMP-30) is added, and continue to surpass
Phonoresponse 1h.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven, obtain resin-rubber slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Embodiment 4
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
80 DEG C of temperature reaction 1h under gas atmosphere, then washs precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
The mass ratio for preparing epoxy resin (E-51), curing agent (MeTHPA) and liquid XNBR is 100:70:
11 resin-rubber solutions, the multi-walled carbon nanotube that equal proportion adds 2.0wt% (1.0wt% respectively) arrive with modified graphene
In resin system solution.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator (DMP-30) is added, and continue to surpass
Phonoresponse 1h.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven, obtain resin-rubber slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Embodiment 5
The present embodiment and the difference of embodiment 1 are that the matrix used in the present embodiment is to add 100 parts of epoxies
Resin (E-51) and 35 parts of curing agent MDAs (DDM), it is well mixed, then adds 11 parts of liquid carboxyl butyronitrile rubbers
The well mixed matrix liquid formed of glue.
Embodiment 6
The present embodiment and the difference of embodiment 2 are that the matrix used in the present embodiment is to add 100 parts of epoxies
Resin (E-51) and 35 parts of curing agent MDAs (DDM), it is well mixed, then adds 11 parts of liquid carboxyl butyronitrile rubbers
The well mixed matrix liquid formed of glue.
Embodiment 7
The present embodiment and the difference of embodiment 3 are that the matrix used in the present embodiment is to add 100 parts of epoxies
Resin (E-51) and 35 parts of curing agent MDAs (DDM), it is well mixed, then adds 11 parts of liquid carboxyl butyronitrile rubbers
The well mixed matrix liquid formed of glue.
Embodiment 8
The present embodiment and the difference of embodiment 4 are that the matrix used in the present embodiment is to add 100 parts of epoxies
Resin (E-51) and 35 parts of curing agent MDAs (DDM), it is well mixed, then adds 11 parts of liquid carboxyl butyronitrile rubbers
The well mixed matrix liquid formed of glue.
Comparative example 1
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
80 DEG C of temperature reaction 1h under gas atmosphere, then washs precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
The mass ratio for preparing epoxy resin (E-51), curing agent (MeTHPA) and liquid XNBR is 100:70:
11 resin-rubber solutions.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator (DMP-30) is added, and after
Continuous ultrasonic reaction 1h.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven, obtain resin-rubber
Slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Comparative example 2
Weigh NaNO3Solid 1.5g, crystalline flake graphite 1.5g, KMnO49g is stand-by, NaNO3Solid is dissolved in the 100ml concentrated sulfuric acids
In, it is placed in ice-water bath and adds rotor and be stirred continuously addition native graphite, persistently stirs 30min；It is slowly added to KMnO4, hold
It is continuous 0 DEG C, continue to stir 30min.35 DEG C are then heated to, stirs 1h；138ml deionized waters are added (in 10min slowly to add
Enter) 98 DEG C are then heated to, keep 15min in the temperature；The deionized water that 420ml is preheating to 50 DEG C in advance is added, is added
43ml hydrogen peroxide, terminating reaction, and 10min is stirred until no longer producing bubble；Configuration about 5% hydrochloric acid solution (600ml go from
Sub- water+100ml concentrated hydrochloric acids), it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugation
Liquid pH=7, then freeze precipitation and obtain graphene oxide, take gained graphene oxide, be quickly put into and be preheated to 1050 DEG C
30s expanded graphite alkene is kept in Muffle furnace；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains stone
Black alkene；
100mg graphenes are dissolved in the uniform dispersion that 0.33mg/mL is formed in 300mL dimethylformamides, are added dropwise
The dimethyl formamide solution of 0.01mol isocyanates is into above-mentioned graphene dispersing solution and continues to stir, and mixed solution is in nitrogen
80 DEG C of temperature reaction 1h under gas atmosphere, then washs precipitation 2 times with dimethylformamide, the addition 0.05mol the third two into precipitation
The dimethyl formamide solution of aldehyde simultaneously continues to stir 55 DEG C of one nights of reaction of keeping temperature, finally by centrifugation, dimethylformamide
Washing, vacuum drying obtain modified graphene；
Prepare epoxy resin (E-51), the quality of curing agent MDA (DDM) and liquid XNBR
Than for 100:35:11 resin-rubber solutions.Then, after mechanical agitation and ultrasonic reaction 6h, 0.6mL accelerator is added
(DMP-30), and ultrasonic reaction 1h is continued.Then, place reaction liquid into and be preheated to de-bubbled 0.5h in 50 DEG C of vacuum drying oven,
Obtain resin-rubber slurries；
Resin rubber slurries are poured into steeping vat, and supersonic generator is placed in steeping vat, control operating power
In 150W；It is 10s to control the impregnation time, and tow tension is 180 grams, is passed through after expanding T300 level 3K carbon fiber impregnations using Weihai
Row's silk machine arranges silk by the way of winding, winds 3 layers repeatedly altogether, forms unidirectional prepreg cloth, prepreg cloth is removed, true at 60 DEG C
10h is dried under empty condition.Then 5h is dried at 120 DEG C, obtains carbon fiber/graphite alkene/CNT/resin prepreg material.
Prepreg is prepared into laminate by hot press, pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130
DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon fiber/graphite alkene/CNT/epoxy of the present invention
Resin composite materials.
Test
Composite in whole embodiments and comparative example is cut to required for testing standard using diamond cutter
Size, according to《GB/T 1447-2005》The tensile strength of standard testing composite, according to《JC/T773-2010》Standard is surveyed
Interlaminar shear strength is tried, test result is as shown in table 1.
This it appears that adding carbon fiber/graphite alkene/CNT/ring of modified graphene/CNT from table
Tensile strength and interlaminar shear strength the ratio comparative example of epoxy resin composite material are high, and comparative example is not add modified graphene/carbon
Nanotube carbon fiber resin matrix composite.The carbon material of addition modified graphene/more sizes of CNT is indicated compound
Load can be effectively transmitted in material matrix, improves the mechanical property of composite.
Table 1
| Sample | Tensile strength (MPa) | Interlaminar shear strength (MPa) |
| Embodiment 1 | 51.97 | 81.28 |
| Embodiment 2 | 55.91 | 83.63 |
| Embodiment 3 | 60.02 | 87.80 |
| Embodiment 4 | 63.53 | 82.17 |
| Embodiment 5 | 52.79 | 82.01 |
| Embodiment 6 | 56.71 | 84.35 |
| Embodiment 7 | 60.82 | 87.90 |
| Embodiment 8 | 64.31 | 82.89 |
| Comparative example 1 | 52.63 | 79.81 |
| Comparative example 2 | 52.45 | 79.54 |
Claims (7)
1. a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg, it is characterised in that include successively
Following steps：
Step 1：Prepare graphene
Step 2：Graphene is dissolved in the uniform dispersion that 0.1-1mg/mL is formed in dimethylformamide, isocyanic acid is added dropwise
The dimethyl formamide solution of ester is into above-mentioned graphene dispersing solution and continues to stir, mixed solution in a nitrogen atmosphere, 75-80
DEG C reaction 1h, then wash precipitation with dimethylformamide, into precipitation addition MDA dimethyl formamide solution and hold
At continuous 55 DEG C of one nights of reaction of stirring keeping temperature, finally by centrifugation, dimethylformamide washing, vacuum drying obtains modified graphite
Alkene；
Step 3：The mass ratio for preparing epoxy resin, curing agent MeTHPA and liquid XNBR is 100:60-80:8-
The quality of 12 resin-rubbery system and epoxy resin, curing agent MDA (DDM) and liquid XNBR
Than for 100:30-40:8-12 resin-rubbery system, then add multi-walled carbon nanotube and modified graphene, multi-wall carbon nano-tube
Pipe is equal with the addition quality of modified graphene, and weight/mass percentage composition is 0.05wt%-1.0wt%；Then, mechanical agitation is simultaneously
After ultrasonic reaction 5-7h, (dimethylamino methyl) phenol (DMP-30) of accelerator 2,4,6- tri- is added, and continue ultrasonic reaction 1h；
Then, place reaction liquid into and be preheated to de-bubbled at least 0.5h in 50 DEG C of vacuum drying oven, obtain modified graphene/carbon nanometer
Pipe/epoxy resin slurry；
Step 4：Modified graphene/carbon nano tube/epoxy resin slurry is poured into steeping vat, and places and surpasses in steeping vat
Sonic generator, carbon fiber is immersed in modified graphene/carbon nano tube/epoxy resin slurry, passes through one after the completion of impregnation
Spreading roller removes unnecessary resin adhesive liquid；
Step 5：Tow after impregnation arranges silk by way of arranging silk machine using winding, is wound repeatedly, forms unidirectional preimpregnation
Cloth；
Step 6：Prepreg cloth is removed, 7-12h is dried under 50-70 DEG C of vacuum condition；Then 4-6h is dried at 100-120 DEG C,
Obtain carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg.
2. according to a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg described in claim 1,
Characterized in that, prepare graphene：Weigh NaNO3Solid is dissolved in 98% concentrated sulfuric acid, is placed in ice-water bath and is added rotor not
Disconnected stirring, adds crystalline flake graphite, persistently stirs 30min, be slowly added to KMnO4, kept for 0 DEG C, continue to stir 30min.Then rise
Temperature stirs 1h to 35 DEG C；Add deionized water and then heat to 98 DEG C, 15min is kept in the temperature；Addition is preheating to 50 in advance
DEG C deionized water, add hydrogen peroxide, terminating reaction, and stir 10min until no longer produce bubble；The hydrochloric acid of preparation 5% is molten
Liquid, it is added in reaction solution, centrifugation is precipitated；Washed repeatedly with deionized water and be precipitated to centrifugate pH=7, gained is sunk
Form sediment it is lyophilized obtains graphene oxide, take gained graphene oxide, be quickly put into be preheated in 1050 DEG C of Muffle furnace and keep 30
Second expanded graphite alkene；A certain amount of expanded graphite alkene is taken to add in absolute ethyl alcohol, ultrasound peels off 15h, obtains graphene.
3. according to a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg described in claim 1,
Characterized in that, in step 2, graphene：Isocyanates：MDA uses magnitude relation 100mg：0.005-0.1mol：0.05-
0.1mol。
4. according to a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg described in claim 1,
Characterized in that, graphene is dissolved in the uniform dispersion that 0.33mg/mL is formed in dimethylformamide.
5. according to a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg described in claim 1,
Characterized in that, epoxy resin is E-51.
6. according to a kind of preparation method of carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg described in claim 1,
Characterized in that, in step 4, control operating power is in 120-170W；It is 8-15s, tow tension 160- to control the impregnation time
200 grams.
7. a kind of carbon fiber/graphite alkene/carbon nano tube/epoxy resin composite material, it is characterised in that appoint claim 1-6
Carbon fiber/graphite alkene/carbon nano tube/epoxy resin prepreg prepares laminate by hot press obtained by one preparation method,
Pressure used is 5MPa, and temperature-rise period is：90 DEG C, 1h；130 DEG C, 2h；150 DEG C, 2h, then pressurize is cooled to room temperature and obtains carbon
Fiber/graphene/carbon nano-tube/epoxy resin composite material.
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