CN107903627A - A kind of thermoplasticity lightweight composite material and preparation method thereof - Google Patents
A kind of thermoplasticity lightweight composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C08K7/14—Glass
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention discloses a kind of thermoplasticity lightweight composite material and preparation method thereof, belong to technical field of composite materials.The thermoplasticity lightweight composite material includes the component of following parts by weight：15 20 parts of 20 30 parts of modified carbon fiber, 80 84 parts of polyimide powder, 10 15 parts of modified glass-fiber, 10 12 parts of heat stabilizer and antioxidant.The thermoplasticity lightweight composite material is by the material composition with special formulation content, under the mutual synergistic effect of these materials, obtained thermoplasticity lightweight composite material interface compatibility, bonding force, intensity and firmness is set to be greatly enhanced, and as a result of quality relative to the lighter polyimides of metal material, whole composite material is light, has a vast market prospect.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of thermoplasticity lightweight composite material.
Background technology
Application of the advanced composite material in Aeronautics and Astronautics industry shows unique advantage and potentiality, from asphalt mixtures modified by epoxy resin
Fat, thermoplastic resin, isocyanate resin to bimaleimide resin, the development course of polyimide resin.Polyimides
Comprehensive performance is very excellent, has very excellent heat resistance, lower temperature resistance, solvent resistance, self lubricity and the spy such as fire-retardant
Property, application is quite varied.
Since materials application environment is increasingly harsh, the performance requirement of composite material is also improved therewith, especially material
Mechanical property.Although current polyimide-based composite material disclosure satisfy that the demand of product heat resistance, intensity need
Further improve.In the process of polyimide-based composite material, correctly formula and additive are selected, is made it have excellent
Different thermoplasticity and mechanical property is most important.In order to improve the mechanical property of composite material, often increase fiber in the base,
Such as carbon fiber, plant fiber, by fibre reinforced matrix intensity, since polyimide matrix is organic material and inorfil
Fusion, its polarity spectrum is larger, and problem occurs in both compatibilities and dispersiveness, can reduce the original intensity of matrix on the contrary.This
A little factors all restrict the development of advanced composite material.
The content of the invention
It is existing in order to solve the problems, such as, it is an object of the invention to provide a kind of thermoplasticity lightweight composite material,
Light weight, intensity are high, thermoplasticity is good.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
A kind of thermoplasticity lightweight composite material, includes the component of following parts by weight：20-30 parts of modified carbon fiber, polyamides
15-20 parts of 80-84 parts of imines powder, 10-15 parts of modified glass-fiber, 10-12 parts of heat stabilizer and antioxidant；
Wherein, the preparation method of modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense nitre
Graphene after sour acidification carries out graft reaction with silane coupling agent, modified graphene is made, by modified graphene, 4,5-
7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Starch agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, it is fine that carbon modified is made
Dimension；
Wherein, the preparation method of modified glass-fiber is：After glass fibre ultrasonic cleaning, in 125-130 DEG C of bar
Dried under part, then add in silane coupling agent and stir 5-10min, dried under conditions of being placed in 80-100 DEG C, modified glass is made
Glass fiber.
Further, in preferred embodiments of the present invention, preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 4-5h in the concentrated sulfuric acid, is placed in magnetic in concentrated nitric acid again after ultrasonic cleaning 1.5-2h
Power stirs 50-60min, and constant temperature reflux 2-3h, is diluted and filtered with deionized water, by filtrate under conditions of 100-120 DEG C
Cleaned repeatedly with deionized water until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 55-60 DEG C, makes
Obtain acidifying graphite alkene；
It is 4.8-5.2 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to
Solute mass fraction is 2.5% mixed solution, and it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite
Alkene, after ultrasonic disperse 30min, the mechanical agitation 2-3h under the conditions of temperature is 75-80 DEG C of water bath with thermostatic control, obtained reactant is used
Acetone cleaning after be filtered by vacuum, then with washes of absolute alcohol until filtrate pH value be 7, the vacuum drying under conditions of 85-90 DEG C,
Modified graphene is made.
Further, in preferred embodiments of the present invention, above-mentioned thermoplasticity lightweight composite material is included by weight
10 parts of 15 parts of 80 parts of 25 parts of modified carbon fiber, polyimide powder, modified glass-fiber, the heat stabilizer and antioxidant 15 of meter
Part.
The preparation method of above-mentioned thermoplasticity lightweight composite material, including：Fallen after according to said ratio, raw material is mixed
Enter in mould, handle 1.5-2h under conditions of temperature is 260-280 DEG C, pressure is 10-12MPa, be then warming up to 340- again
350 DEG C of processing 1.5-2h, demould after being cooled to 100 DEG C, composite material are made.
The invention has the advantages that：
The present invention is using polyimide powder as material matrix, using modified carbon fiber and modified glass-fiber as reinforcement, leads to
Cross and processing be modified to existing carbon fiber and glass fibre so that modified carbon fiber and glass fibre with it is polyimide-based
Body merges well, solves the problems, such as that the interfacial combined function between carbon fiber and matrix is poor, improves polyimides material
The mechanical property of material.
The present invention carries out graft modification to existing carbon fiber, with existing graft modification the difference is that the present invention is not pair
Carbon fiber directly carries out grafting processing, but by the way that graphene and silane coupling agent are carried out graft reaction, modified graphite is made
Alkene, then again with modified graphene, 4,5- 7-oxa-bicyclo[4.1.0s -1,2- dicarboxylic acid diglycidyl ester and curing agent according to weight ratio
For 3:55:10 ratio mixing, is made sizing agent, then by sizing agent coated on carbon fiber, and under an inert atmosphere with penetrating
Line finally obtains modified carbon fiber according to the dose delivery of 240kGy.
During modified carbon fiber is prepared, modified graphene has the functional group for being easy to merge with matrix, and
On the one hand its surface forms active function groups, these active function groups to graphene after the concentrated sulfuric acid and concentrated nitric acid acidification
Reactivity can be improved, make more silane coupling agents and graphene that graft reaction occur, on the other hand by the concentrated sulfuric acid and
Concentrated nitric acid is etched graphene surface, improves graphene surface roughness, increases specific surface area so that graphene can be with
Silane coupling agent realizes mechanical interlock, so that the sizing agent as made from modified graphene can help carbon fiber and base
Body polyimides preferably merges.By being modified processing to graphene so that sizing agent can be tied well with carbon fiber
The problem of closing, overcoming sizing agent and poor carbon fiber Tuberculous.
For the wetability of further modified carbon fiber in the base, the present invention bombards carbon fiber surface by x ray irradiation x
Face, on the one hand produces chemical reactivity free radical or grafting active function groups so that carbon fiber can be with carbon fiber surface
Matrix produces chemical bonding, so as to improve the wetability of carbon fiber in the base, while also further increase silane coupling agent with
The reactivity of 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and carbon fiber；On the other hand x ray irradiation x is passed through
Carbon fiber surface is etched, increased fiber roughness, improves the mechanical locking force between carbon fiber and basal body interface, and then make
The boundary strength for obtaining whole composite material is improved.Ray of the invention signified can be X-ray, gamma-rays, electron beam or
Ultraviolet etc..
The present invention is also added with the same glass fibre with enhancing effect on the basis of addition modified carbon fiber,
Glass fibre has the advantages such as cheap and elongation percentage is big in itself, can effectively make up that carbon fiber ductility rate is low and price is held high
Your the defects of.Two kinds of fibrous materials are mutually brought out one's strengths to make up for one's weaknesses, and on the premise of bearing capacity is ensured, are improved material ductility and are reduced
Cost.Meanwhile the glass fibre that the present invention uses is also by modification, by with silane coupling agent be grafted instead
Should so that modified glass-fiber can preferably be merged with matrix, and it is dispersed in the base.
The thermoplasticity lightweight composite material of the present invention is by the material composition with special formulation content, in these materials
Mutually under synergistic effect, obtain obtained thermoplasticity lightweight composite material interface compatibility, bonding force, intensity and firmness
Greatly improve, and as a result of quality relative to the lighter polyimides of metal material, whole composite material is light, has
Vast market prospect.
Embodiment
The principle of the present invention and feature are described with reference to embodiments, the given examples are served only to explain the present invention,
It is not intended to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, suggests according to normal condition or manufacturer
Condition carries out.Reagents or instruments used without specified manufacturer, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1：
The thermoplasticity lightweight composite material of the present embodiment includes the component of following parts by weight：20 parts of modified carbon fiber, gather
15 parts of 84 parts of imide powder, 10 parts of modified glass-fiber, 10 parts of heat stabilizer and antioxidant.
(1) preparation method of above-mentioned modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense
Graphene after nitric acid acidification carries out graft reaction with silane coupling agent, and modified graphene is made, by modified graphene, 4,
5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Sizing agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, carbon modified is made
Fiber.
Preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 4h in the concentrated sulfuric acid, magnetic force in concentrated nitric acid is placed in again after ultrasonic cleaning 1.5h and stirs
60min is mixed, constant temperature reflux 2h, is diluted and filtered with deionized water, by filtrate with deionized water repeatedly under conditions of 120 DEG C
Until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 55 DEG C, is made acidifying graphite alkene for cleaning.
It is 4.8 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to solute
Mass fraction is 2.5% mixed solution, and it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite alkene, surpasses
After sound disperses 30min, the mechanical agitation 2h under the conditions of temperature is 80 DEG C of water bath with thermostatic control, after obtained reactant is cleaned with acetone
Vacuum filtration, then with washes of absolute alcohol until filtrate pH value is 7, the vacuum drying under conditions of 85 DEG C, is made modified graphite
Alkene.
(2) preparation method of above-mentioned modified glass-fiber is：After glass fibre ultrasonic cleaning, in 125 DEG C of condition
Lower drying, then adds in silane coupling agent and stirs 10min, dried under conditions of being placed in 80 DEG C, modified glass-fiber is made.
The preparation method of the thermoplasticity lightweight composite material of the present embodiment, including：Raw material is mixed according to said ratio
After pour into mould, handle 1.5h under conditions of temperature is 260 DEG C, pressure is 12MPa, be then warming up to 340 DEG C of processing again
1.5h, demoulds after being cooled to 100 DEG C, and composite material is made.
Embodiment 2：
The thermoplasticity lightweight composite material of the present embodiment includes the component of following parts by weight：30 parts of modified carbon fiber, gather
20 parts of 80 parts of imide powder, 15 parts of modified glass-fiber, 12 parts of heat stabilizer and antioxidant.
(1) preparation method of above-mentioned modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense
Graphene after nitric acid acidification carries out graft reaction with silane coupling agent, and modified graphene is made, by modified graphene, 4,
5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Sizing agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, carbon modified is made
Fiber.
Preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 5h in the concentrated sulfuric acid, is placed in magnetic agitation in concentrated nitric acid again after ultrasonic cleaning 2h
60min, constant temperature reflux 3h, is diluted and filtered with deionized water under conditions of 120 DEG C, and filtrate is repeatedly clear with deionized water
Wash until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 60 DEG C, is made acidifying graphite alkene.
It is 5.2 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to solute
Mass fraction is 2.5% mixed solution, and it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite alkene, surpasses
After sound disperses 30min, the mechanical agitation 3h under the conditions of temperature is 75 DEG C of water bath with thermostatic control, after obtained reactant is cleaned with acetone
Vacuum filtration, then with washes of absolute alcohol until filtrate pH value is 7, the vacuum drying under conditions of 90 DEG C, is made modified graphite
Alkene.
(2) preparation method of above-mentioned modified glass-fiber is：After glass fibre ultrasonic cleaning, in 130 DEG C of condition
Lower drying, then adds in silane coupling agent and stirs 5min, dried under conditions of being placed in 100 DEG C, modified glass-fiber is made.
The preparation method of the thermoplasticity lightweight composite material of the present embodiment, including：Raw material is mixed according to said ratio
After pour into mould, handle 2h under conditions of temperature is 280 DEG C, pressure is 10MPa, be then warming up to again 350 DEG C processing 2h,
Demoulded after being cooled to 100 DEG C, composite material is made.
Embodiment 3：
The thermoplasticity lightweight composite material of the present embodiment includes the component of following parts by weight：25 parts of modified carbon fiber, gather
28 parts of 82 parts of imide powder, 12 parts of modified glass-fiber, 11 parts of heat stabilizer and antioxidant.
(1) preparation method of above-mentioned modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense
Graphene after nitric acid acidification carries out graft reaction with silane coupling agent, and modified graphene is made, by modified graphene, 4,
5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Sizing agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, carbon modified is made
Fiber.
Preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 4.5h in the concentrated sulfuric acid, is placed in magnetic force in concentrated nitric acid again after ultrasonic cleaning 1.6h
55min is stirred, constant temperature reflux 2.5h, is diluted and filtered with deionized water, by filtrate deionized water under conditions of 110 DEG C
Until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 58 DEG C, is made acidifying graphite alkene for cleaning repeatedly；
Dilute hydrochloric acid solution adjusting pH value is added into absolute ethyl alcohol and is configured to Solute mass for 5 and then addition silane coupling agent
Fraction is 2.5% mixed solution, and it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite alkene, ultrasound point
After dissipating 30min, the mechanical agitation 2.4h under the conditions of temperature is 77 DEG C of water bath with thermostatic control is true after obtained reactant is cleaned with acetone
Sky filters, then with washes of absolute alcohol until filtrate pH value is 7, the vacuum drying under conditions of 88 DEG C, is made modified graphene.
(2) preparation method of above-mentioned modified glass-fiber is：After glass fibre ultrasonic cleaning, in 128 DEG C of condition
Lower drying, then adds in silane coupling agent and stirs 8min, dried under conditions of being placed in 90 DEG C, modified glass-fiber is made.
The preparation method of the thermoplasticity lightweight composite material of the present embodiment, including：Raw material is mixed according to said ratio
After pour into mould, handle 1.8h under conditions of temperature is 270 DEG C, pressure is 11MPa, be then warming up to 345 DEG C of processing again
1.8h, demoulds after being cooled to 100 DEG C, and composite material is made.
Embodiment 4：
The thermoplasticity lightweight composite material of the present embodiment includes the component of following parts by weight：25 parts of modified carbon fiber, gather
15 parts of 80 parts of imide powder, 15 parts of modified glass-fiber, 10 parts of heat stabilizer and antioxidant.
(1) preparation method of above-mentioned modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense
Graphene after nitric acid acidification carries out graft reaction with silane coupling agent, and modified graphene is made, by modified graphene, 4,
5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Sizing agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, carbon modified is made
Fiber；
Preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 5h in the concentrated sulfuric acid, is placed in magnetic agitation in concentrated nitric acid again after ultrasonic cleaning 2h
50min, constant temperature reflux 3h, is diluted and filtered with deionized water under conditions of 105 DEG C, and filtrate is repeatedly clear with deionized water
Wash until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 60 DEG C, is made acidifying graphite alkene；
It is 5 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to solute matter
The mixed solution that fraction is 2.5% is measured, it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite alkene, ultrasound
After scattered 30min, the mechanical agitation 3h under the conditions of temperature is 80 DEG C of water bath with thermostatic control is true after obtained reactant is cleaned with acetone
Sky filters, then with washes of absolute alcohol until filtrate pH value is 7, the vacuum drying under conditions of 90 DEG C, is made modified graphene.
(2) preparation method of above-mentioned modified glass-fiber is：After glass fibre ultrasonic cleaning, in 130 DEG C of condition
Lower drying, then adds in silane coupling agent and stirs 6min, dried under conditions of being placed in 95 DEG C, modified glass-fiber is made.
The preparation method of the thermoplasticity lightweight composite material of the present embodiment, including：Raw material is mixed according to said ratio
After pour into mould, handle 1.5h under conditions of temperature is 275 DEG C, pressure is 11.5MPa, be then warming up to again at 345 DEG C
1.5h is managed, is demoulded after being cooled to 100 DEG C, composite material is made.
Embodiment 5：
The thermoplasticity lightweight composite material of the present embodiment includes the component of following parts by weight：28 parts of modified carbon fiber, gather
18.6 parts of 83 parts of imide powder, 14 parts of modified glass-fiber, 10.5 parts of heat stabilizer and antioxidant.
(1) preparation method of above-mentioned modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense
Graphene after nitric acid acidification carries out graft reaction with silane coupling agent, and modified graphene is made, by modified graphene, 4,
5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Sizing agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, carbon modified is made
Fiber；
Preparing modified graphene includes step in detail below：
Graphene is placed in magnetic agitation 4.5h in the concentrated sulfuric acid, magnetic force in concentrated nitric acid is placed in again after ultrasonic cleaning 2h and stirs
60min is mixed, constant temperature reflux 3h, is diluted and filtered with deionized water, by filtrate with deionized water repeatedly under conditions of 120 DEG C
Until filtrate pH value is 7, vacuum drying under conditions of filtrate then is placed in 55 DEG C, is made acidifying graphite alkene for cleaning；
It is 5 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to solute matter
The mixed solution that fraction is 2.5% is measured, it is 1 that solid-liquid ratio is pressed into mixed solution:1 weight ratio adds acidifying graphite alkene, ultrasound
After scattered 30min, the mechanical agitation 2.5h under the conditions of temperature is 80 DEG C of water bath with thermostatic control, after obtained reactant is cleaned with acetone
Vacuum filtration, then with washes of absolute alcohol until filtrate pH value is 7, the vacuum drying under conditions of 90 DEG C, is made modified graphite
Alkene.
(2) preparation method of above-mentioned modified glass-fiber is：After glass fibre ultrasonic cleaning, in 128 DEG C of condition
Lower drying, then adds in silane coupling agent and stirs 9min, dried under conditions of being placed in 95 DEG C, modified glass-fiber is made.
The preparation method of the thermoplasticity lightweight composite material of the present embodiment, including：Raw material is mixed according to said ratio
After pour into mould, handle 2h under conditions of temperature is 265 DEG C, pressure is 12MPa, be then warming up to 350 DEG C of processing again
1.5h, demoulds after being cooled to 100 DEG C, and composite material is made.
Test example
By above-described embodiment 1-5 and comparative example 1 (comparative example according to existing composite polyimide material preparation method
Be made) prepare thermoplasticity lightweight composite material sample is made with injection molding machine, according to GB2568-1995 test pour mass drawing
Performance is stretched, according to the interlaminar shear strength of JC/T773-1996 test tablet unidirectional composite materials, test data such as table 1 below：
Table 1
| Embodiment | Tensile strength/MPa | Ultimate strength/N | Stretch modulus/MPa | Interlaminar shear strength/MPa |
| 1 | 5098.78 | 2249.56 | 285134.78 | 5112.56 |
| 2 | 5123.45 | 2254.21 | 285795.46 | 5125.12 |
| 3 | 5126.76 | 2268.34 | 285924.51 | 5124.79 |
| 4 | 5131.07 | 2276.31 | 286371.84 | 5128.34 |
| 5 | 5125.16 | 2248.97 | 285789.47 | 5126.35 |
| Comparative example | 4256.48 | 1950.83 | 248096.36 | 4257.89 |
The more common wood and plastic composite of thermoplasticity lightweight composite material produced by the present invention it can be seen from upper table data
Tensile strength, ultimate strength, stretch modulus and the interlaminar shear strength of material are all significantly improved, this is greatly expanded
The application range of the thermoplasticity lightweight composite material of the present invention, has great development prospect.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of thermoplasticity lightweight composite material, it is characterised in that include the component of following parts by weight：Modified carbon fiber 20-
15-20 parts of 30 parts, 80-84 parts of polyimide powder, 10-15 parts of modified glass-fiber, 10-12 parts of heat stabilizer and antioxidant；
Wherein, the preparation method of the modified carbon fiber is：Carbon fiber is subjected to cleaning removal of impurities processing；Will be through the concentrated sulfuric acid and dense nitre
Graphene after sour acidification carries out graft reaction with silane coupling agent, modified graphene is made, by modified graphene, 4,5-
7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters and curing agent are 3 according to weight ratio:55:10 ratio mixing, is made
Starch agent；Carbon fiber is placed in sizing agent the dose delivery with ray according to 240kGy under an inert atmosphere, the modification is made
Carbon fiber；
Wherein, the preparation method of the modified glass-fiber is：After glass fibre ultrasonic cleaning, in 125-130 DEG C of bar
Dried under part, then add in silane coupling agent and stir 5-10min, dried under conditions of being placed in 80-100 DEG C, be made described and change
Property glass fibre.
2. thermoplasticity lightweight composite material according to claim 1, it is characterised in that prepare the modified graphene bag
Include step in detail below：
Graphene is placed in magnetic agitation 4-5h in the concentrated sulfuric acid, magnetic force in concentrated nitric acid is placed in again after ultrasonic cleaning 1.5-2h and stirs
50-60min is mixed, constant temperature reflux 2-3h, is diluted and filtered with deionized water, filtrate is spent under conditions of 100-120 DEG C
Ionized water cleans repeatedly until filtrate pH value is 7, and vacuum drying under conditions of filtrate then is placed in 55-60 DEG C, is made acid
Graphite alkene；
It is 4.8-5.2 that dilute hydrochloric acid solution is added into absolute ethyl alcohol and adjusts pH value, then adds silane coupling agent and is configured to solute
Mass fraction is 2.5% mixed solution, and it is 1 that solid-liquid ratio is pressed into the mixed solution:1 weight ratio adds acidifying graphite
Alkene, after ultrasonic disperse 30min, the mechanical agitation 2-3h under the conditions of temperature is 75-80 DEG C of water bath with thermostatic control, obtained reactant is used
Acetone cleaning after be filtered by vacuum, then with washes of absolute alcohol until filtrate pH value be 7, the vacuum drying under conditions of 85-90 DEG C,
Modified graphene is made.
3. thermoplasticity lightweight composite material according to claim 1 or 2, it is characterised in that the thermoplasticity lightweight
Composite material includes 15 parts of 80 parts of 25 parts of modified carbon fiber, polyimide powder, modified glass-fiber by weight, thermostabilization
15 parts of 10 parts of agent and antioxidant.
4. the preparation method of claim 1-3 any one of them thermoplasticity lightweight composite materials, it is characterised in that including：
Pour into mould after raw material is mixed according to said ratio, locate under conditions of temperature is 260-280 DEG C, pressure is 10-12MPa
1.5-2h is managed, 340-350 DEG C of processing 1.5-2h is then warming up to again, is demoulded after being cooled to 100 DEG C, the composite material is made.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233109A (en) * | 2018-10-15 | 2019-01-18 | 江西江铃集团奥威汽车零部件有限公司 | A kind of foamed material of automotive seat and its preparation method and application |
| CN109504086A (en) * | 2018-10-10 | 2019-03-22 | 安徽省科晟生态木装饰材料有限公司 | A kind of preparation method of bamboo carbon fibre composite polyimide material |
| CN110435239A (en) * | 2019-06-28 | 2019-11-12 | 东华大学 | Multiple dimensioned epoxy resin toughened base carbon fiber composite material of one kind and preparation method thereof |
| CN110643076A (en) * | 2019-08-14 | 2020-01-03 | 浙江海洋大学 | Preparation method of transparent substrate film of flexible electronic device |
| CN110861319A (en) * | 2019-11-20 | 2020-03-06 | 中广核高新核材科技（苏州）有限公司 | Radiation-resistant high-temperature-resistant fiber composite material and preparation method thereof |
| CN114589994A (en) * | 2022-03-18 | 2022-06-07 | 江苏悦达绿色建筑科技有限公司 | Building material with heat-preservation glass fiber composite structure, production device and production method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181152A (en) * | 2011-03-30 | 2011-09-14 | 同济大学 | Preparation method for multidimensional mixed composite mateial of carbon fiber/polyimide resin modified by carbon nano tube |
| CN102787488A (en) * | 2012-07-30 | 2012-11-21 | 哈尔滨工业大学 | Method for preparing graphene oxide grafting surface modification carbon fiber |
| CN105713386A (en) * | 2014-11-30 | 2016-06-29 | 黑龙江鑫达企业集团有限公司 | Carbon fiber-reinforced thermoplastic polyimide composite material |
| CN105968718A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation method of carbon fiber/graphene/epoxy resin prepreg and carbon fiber composite material |
-
2017
- 2017-11-29 CN CN201711227771.4A patent/CN107903627A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181152A (en) * | 2011-03-30 | 2011-09-14 | 同济大学 | Preparation method for multidimensional mixed composite mateial of carbon fiber/polyimide resin modified by carbon nano tube |
| CN102787488A (en) * | 2012-07-30 | 2012-11-21 | 哈尔滨工业大学 | Method for preparing graphene oxide grafting surface modification carbon fiber |
| CN105713386A (en) * | 2014-11-30 | 2016-06-29 | 黑龙江鑫达企业集团有限公司 | Carbon fiber-reinforced thermoplastic polyimide composite material |
| CN105968718A (en) * | 2016-05-20 | 2016-09-28 | 北京化工大学 | Preparation method of carbon fiber/graphene/epoxy resin prepreg and carbon fiber composite material |
Non-Patent Citations (1)
| Title |
|---|
| 陈照峰: "《无机非金属材料学》", 29 February 2016, 西北工业大学出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504086A (en) * | 2018-10-10 | 2019-03-22 | 安徽省科晟生态木装饰材料有限公司 | A kind of preparation method of bamboo carbon fibre composite polyimide material |
| CN109233109A (en) * | 2018-10-15 | 2019-01-18 | 江西江铃集团奥威汽车零部件有限公司 | A kind of foamed material of automotive seat and its preparation method and application |
| CN110435239A (en) * | 2019-06-28 | 2019-11-12 | 东华大学 | Multiple dimensioned epoxy resin toughened base carbon fiber composite material of one kind and preparation method thereof |
| CN110435239B (en) * | 2019-06-28 | 2021-11-09 | 东华大学 | Multi-scale toughened epoxy resin-based carbon fiber composite material and preparation method thereof |
| CN110643076A (en) * | 2019-08-14 | 2020-01-03 | 浙江海洋大学 | Preparation method of transparent substrate film of flexible electronic device |
| CN110861319A (en) * | 2019-11-20 | 2020-03-06 | 中广核高新核材科技（苏州）有限公司 | Radiation-resistant high-temperature-resistant fiber composite material and preparation method thereof |
| CN114589994A (en) * | 2022-03-18 | 2022-06-07 | 江苏悦达绿色建筑科技有限公司 | Building material with heat-preservation glass fiber composite structure, production device and production method |
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