CN109206905A - A kind of graphene bismaleimide resin composite material and preparation method thereof - Google Patents
A kind of graphene bismaleimide resin composite material and preparation method thereof Download PDFInfo
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- CN109206905A CN109206905A CN201810994027.5A CN201810994027A CN109206905A CN 109206905 A CN109206905 A CN 109206905A CN 201810994027 A CN201810994027 A CN 201810994027A CN 109206905 A CN109206905 A CN 109206905A
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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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The present invention relates to a kind of graphene bismaleimide resin composite materials.It is formed by multi-layer graphene bismaleimide resin prepreg stacking co-curing, and the graphene bismaleimide resin prepreg is combined by the reinforcing material that graphene bismaleimide resin adhesive film and carbon fiber, quartz fibre, glass fibre, aramid fiber and its fabric form.Obtained graphene bismaleimide resin composite material has the characteristics that light-weight, high temperature resistant, mechanical property and electrical and thermal conductivity are good, has extensive use in aerospace, electronic information and high-technology field.
Description
Technical field
The present invention relates to technical field of composite preparation, specifically a kind of graphene bismaleimide resin composite material and
Preparation method.
Background technique
Bismaleimide (BMI) is the bifunctional compound using maleimide as active end group, can with it is a variety of
Copolymer compound is modified as toughness heat stable resin, because its main chain contains aromatic ring and azepine ring structure, assigns this resinoid with resistance to height
A variety of excellent properties such as temperature, wet-heat resisting, radiation hardness, high insulation, rub resistance, fire-retardant, good mechanical properties, good stability of the dimension,
It is widely used in fields such as national defence, aerospace, electronics.Graphene is as a kind of novel nano-material, with carbon nanometer
The materials such as pipe, which are compared, has stable lattice structure and high carrier, has fabulous conductivity, thermal conductivity.Graphite at present
Alkene material is mixed mainly as filler with other components, and electrical property, hot property and other performances, the main method for improving material are
Graphene dispersion is prepared into composite material in other materials, the program is difficult to solve the dispersion of graphene, uses machinery
Method be easy to cause the destruction of graphene, and graphene and basal body interface performance are poor, can only be prepared using solution dispersing method wet
It is good cannot to reach thermal conductivity height, comprehensive mechanical property simultaneously for method prepreg, it is difficult to meet actual needs, limit graphite
The extensive use of alkene material.
Summary of the invention
To solve the above-mentioned technical problems in the prior art, the present invention provides a kind of graphene bismaleimide resin composite wood
Material and preparation method thereof, has the characteristics that light-weight, high temperature resistant, mechanical property and electrical and thermal conductivity are good.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of graphene bismaleimide resin composite material, inside by the prepreg after multi-layer graphene bismaleimide resin and fiber composite
Alternately laminated distribution, modified graphene is uniformly distributed in bismaleimide amine monomer in the graphene bismaleimide resin.
Preferably, the fibrous layer is selected from carbon fiber, quartz fibre, glass fibre, aramid fiber and aforementioned fiber
At least one of fabric.
Preferably, the molar ratio that allyl group is rolled into a ball with dimaleoyl imino in the graphene bismaleimide resin is
1:1~1.2.
Preferably, graphene mass ratio in bismaleimide resin is 0.001%~3%.
Preferably, the resin content of the graphene bismaleimide resin prepreg be 25%~60%, monolayer immobilization with a thickness of
0.01mm~0.45mm.
The preparation method of graphene bismaleimide resin composite material recited above, includes the following steps:
S1 prepares modified graphene；
S2 prepares graphene bismaleimide resin, and modified graphene and bismaleimide amine monomer, modifying agent and toughener is abundant
The graphene bismaleimide resin that mixing dispersion is prepared；
Graphene bismaleimide resin is made on adhesive film machine according to resin content requirement and fiber and reinforcing material surface density by S3
Glue film, it is compound with the progress of carbon fiber, quartz fibre, glass fibre, aramid fiber and its fabric on compounding machine, graphene is made
Bismaleimide resin prepreg；Wherein film thickness is calculated according to resin content and reinforcing material；
S4, according to die size cutting grapheme bismaleimide resin prepreg；The graphene bismaleimide resin prepreg cut is existed
Mold upper layer lay-up patch, obtains composite material blank；
The good composite material ingot solidification of paving is obtained graphene bismaleimide resin composite material by S5.
Preferably, the step S1 is specially that the mixed acid of the concentrated sulfuric acid and concentrated nitric acid is used to carry out at surface graphene
Reason makes its surface generate functional group, mixes after washing is dry with diallyl bisphenol and its homologue or aromatic amine, wherein stone
It is 0.001%~3% that black alkene, which accounts for diallyl bisphenol and its homologue or the mass percent of aromatic amine, and stirring mixture makes it
It is uniformly dispersed, is reacted 2 hours~6 hours in the environment of 120 DEG C~180 DEG C, make diallyl bisphenol and its homologue or virtue
Fragrant amine groups are sufficiently reacted, and obtained diallyl bisphenol graphene mixture is modified graphene.
Preferably, it is 1:1~9 that the concentrated sulfuric acid, which accounts for the volume ratio of concentrated nitric acid, in the mixed acid.
Preferably, in the step S2, mole of allyl group and dimaleoyl imino group in modified graphene
Ratio be 1:1~1.2, the toughener be polysulfones, polyether sulfone, polyether sulphone, polyether-ether-ketone, poly(aryl ether ketone), polyimides or
At least one of polyetherimide, toughener account for the 1%~30% of graphene bismaleimide resin gross mass.
Preferably, flattening graphene bismaleimide resin prepreg, and the prepreg of paving with electric iron in the step S4
Using vacuumizing carry out pre-compacted.
Preferably, curing mode includes autoclave, press, baking oven in the step S5.
After adopting the above technical scheme, technical effect of the invention is as follows:
The compound scheme of the graphene bismaleimide resin and reinforcing fiber layer that are used due to composite material of the present invention, so that
This material has the good electrical and thermal conductivity performance of grapheme material.In addition, using reinforcing fiber in this composite material, strengthen
Fiber specific gravity is small, specific strength and specific modulus are big.Composite material by each component performance complementation and be associated with acquisition single composition material
The inaccessiable comprehensive performance of material institute, specific gravity is small, and specific strength and specific modulus are big, solves existing graphene composite material specific gravity
Greatly, the small equal determination of specific strength, significantly improves material mechanical performance.Graphene span composite material surface electricity of the present invention
Resistance is greater than 1400MPa less than 50 Ω, with T700 grade carbon fiber composite material bending strength, and interlaminar shear strength is greater than 75MPa, draws
Intensity is stretched greater than 1700MPa, and 0 degree of compressive strength is greater than 1050MPa.
Specific embodiment
Combined with specific embodiments below to a kind of graphene bismaleimide resin composite material of the present invention and preparation method thereof make into
One step illustrates, but protection content of the invention is not limited to following embodiment.
Embodiment 1:
The preparation method of the graphene bismaleimide resin composite material containing 8 layers of graphene bismaleimide resin prepreg is prepared, step is such as
Under:
(1) graphene bismaleimide resin T700 one-way fiber prepreg is prepared
(a) preparation of modified graphene
By graphene dispersion in the mixed acid (volume ratio 1:1) of the concentrated sulfuric acid and concentrated nitric acid, ultrasonic reaction 48h under room temperature；Ultrasound
After deionized water be added dropwise dilute concentrated acid solution, when dropwise addition, is stirred continuously.After dilution, washing filtrate to neutrality is done
It is dry.Treated, and graphene in mass ratio 1% is mixed with 99% diallyl bisphenol, makes its dispersion using high-speed stirred method
Uniformly, it is reacted 4 hours in the environment of 150 DEG C, reacts diallyl bisphenol sufficiently with graphene surface group, obtain two
Allyl bisphenol-A graphene mixture；
(b) preparation of graphene bismaleimide resin
Diallyl bisphenol graphene mixture is mixed with bismaleimide monomer, toughener and modifying agent, makes allyl
Group and the molar ratio of dimaleoyl imino group are 1:1, and toughener is polyether sulphone, and toughener ratio is total mass ratio
15%, graphene bismaleimide resin is mixed in equipment；
(c) graphene bismaleimide resin is prepared into glue film, is combined graphene bismaleimide resin prepreg with quartz textile,
Prepreg resin content is 35%, fiber areal densities 133g/m2, thickness in monolayer is 0.125mm after solidification.
(2) according to die size cutting grapheme bismaleimide resin prepreg, 8 layers of graphene bismaleimide resin of paving on mold
Prepreg allows to flatten prepreg with electric iron, allow according to the technological requirements using pre-compacted is vacuumized, according to graphene span
The curing cycle of resin composite materials consolidates the good composite material embryo material of paving using autoclave, press, baking oven or other modes
Change.
(3) graphene bismaleimide resin composite material is obtained after demoulding.
Graphene bismaleimide resin T700 composite material surface resistance is greater than 1400MPa less than 50 Ω, bending strength, and interlayer is cut
Shearing stress is greater than 75MPa, and tensile strength is greater than 1700MPa, and 0 degree of compressive strength is greater than 1050MPa.
Embodiment 2:
The preparation method of the graphene bismaleimide resin composite material containing 16 layers of graphene bismaleimide resin prepreg is prepared, step is such as
Under:
(1) graphene bismaleimide resin glass fabric prepreg is prepared
(a) preparation of modified graphene
By graphene dispersion in the mixed acid (volume ratio 1:9) of the concentrated sulfuric acid and concentrated nitric acid, room temperature removes ultrasonic reaction 48h；It is super
Deionized water is added dropwise after sound to dilute concentrated acid solution, when dropwise addition is stirred continuously.After dilution, washing filtrate to neutrality,
It is dry.Treated, and graphene in mass ratio 3% is mixed with 97% diallyl bisphenol, makes its point using high-speed stirred method
It dissipates uniformly, is reacted 4 hours in the environment of 150 DEG C, react diallyl bisphenol sufficiently with graphene surface group, obtain
Diallyl bisphenol graphene mixture；
(b) preparation of graphene bismaleimide resin
Diallyl bisphenol graphene mixture is mixed with bismaleimide monomer, toughener and modifying agent, makes allyl
Group and the molar ratio of dimaleoyl imino group are 1:1.05, and toughener is polyether sulphone, and toughener ratio is gross mass
The 12% of ratio is mixed with graphene bismaleimide resin in equipment；
(c) graphene bismaleimide resin is prepared into glue film, is combined graphene bismaleimide resin prepreg with quartz textile,
Prepreg resin content is 40%, fiber areal densities 295g/m2, thickness in monolayer is 0.28mm after solidification.
(2) according to die size cutting grapheme bismaleimide resin prepreg, 16 layers of graphene span tree of paving on mold
Rouge prepreg allows to flatten prepreg with electric iron, allows according to the technological requirements using pre-compacted is vacuumized, according to graphene pair
The good composite material embryo material of paving is used autoclave, press, baking oven or other modes by the curing cycle of horse resin composite material
Solidification.
(3) graphene bismaleimide resin composite material is obtained after demoulding.
Graphene span tree glass fiber compound material sheet resistance is greater than 800MPa, interlayer less than 50 Ω, bending strength
Shear strength is greater than 55MPa, and tensile strength is greater than 750MPa, and 0 degree of compressive strength is greater than 650MPa.
Embodiment 3:
The preparation method of the graphene bismaleimide resin composite material containing 4 layers of graphene bismaleimide resin prepreg is prepared, step is such as
Under:
(1) graphene bismaleimide resin quartz textile prepreg is prepared
(a) preparation of modified graphene
By graphene dispersion in the mixed acid (volume ratio 4:6) of the concentrated sulfuric acid and concentrated nitric acid, room temperature removes ultrasonic reaction 48h；It is super
Deionized water is added dropwise after sound to dilute concentrated acid solution, when dropwise addition is stirred continuously.After dilution, washing filtrate to neutrality,
It is dry.The diallyl bisphenol of treated graphene in mass ratio 2% and 93% and 5% diaminodiphenylsulfone mix, using height
Fast stirring means make it be uniformly dispersed, and react 4 hours in the environment of 150 DEG C, make diallyl bisphenol, diaminodiphenylsulfone
It is sufficiently reacted with graphene surface group, obtains graphene mixture；
(b) preparation of graphene bismaleimide resin
Diallyl bisphenol graphene mixture is mixed with bismaleimide monomer, toughener and modifying agent, makes allyl
Group and the molar ratio of dimaleoyl imino group are 1:1, and toughener is polyether sulphone, and toughener ratio is total mass ratio
17%, graphene bismaleimide resin is mixed in equipment；
(c) graphene bismaleimide resin is prepared into glue film, is combined graphene bismaleimide resin prepreg with quartz textile,
Prepreg resin content is 40%, fiber areal densities 125g/m2, thickness in monolayer is 0.12mm after solidification.
(2) according to die size cutting grapheme bismaleimide resin prepreg, 16 layers of graphene span tree of paving on mold
Rouge prepreg allows to flatten prepreg with electric iron, allows according to the technological requirements using pre-compacted is vacuumized, according to graphene pair
The good composite material embryo material of paving is used autoclave, press, baking oven or other modes by the curing cycle of horse resin composite material
Solidification.
(3) graphene bismaleimide resin composite material is obtained after demoulding.
Graphene bismaleimide resin quartz composite material surface resistance is greater than 750MPa less than 50 Ω, bending strength, and interlayer is cut
Shearing stress is greater than 55MPa, and tensile strength is greater than 650MPa, and 0 degree of compressive strength is greater than 600MPa.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (11)
1. a kind of graphene bismaleimide resin composite material, it is characterised in that: by multi-layer graphene bismaleimide resin and fiber inside it
The alternately laminated distribution of prepreg after compound, modified graphene is in bismaleimide amine monomer in the graphene bismaleimide resin
In be uniformly distributed.
2. a kind of graphene bismaleimide resin composite material according to claim 1, it is characterised in that: the fibrous layer is selected from
Carbon fiber, quartz fibre, glass fibre, aramid fiber and aforementioned fiber fabric at least one.
3. a kind of graphene bismaleimide resin composite material according to claim 1, it is characterised in that: the graphene span
The molar ratio of allyl group and dimaleoyl imino group is 1:1~1.2 in resin.
4. a kind of graphene bismaleimide resin composite material according to claim 1, it is characterised in that: the graphene is double
Mass ratio is 0.001%~3% in horse resin.
5. a kind of graphene bismaleimide resin composite material according to claim 1, it is characterised in that: the graphene span
The resin content of resin prepreg material is 25%~60%, and monolayer immobilization is with a thickness of 0.01mm~0.45mm.
6. preparing the preparation method of the described in any item graphene bismaleimide resin composite materials of claim 1-5, it is characterised in that
Include the following steps:
S1 prepares modified graphene；
S2 prepares graphene bismaleimide resin, and modified graphene and bismaleimide amine monomer, modifying agent and toughener is abundant
The graphene bismaleimide resin that mixing dispersion is prepared；
Graphene bismaleimide resin is made on adhesive film machine according to resin content requirement and fiber and reinforcing material surface density by S3
Glue film, it is compound with the progress of carbon fiber, quartz fibre, glass fibre, aramid fiber and its fabric on compounding machine, graphene is made
Bismaleimide resin prepreg；
S4, according to die size cutting grapheme bismaleimide resin prepreg；The graphene bismaleimide resin prepreg cut is existed
Mold upper layer lay-up patch, obtains composite material blank；
The good composite material ingot solidification of paving is obtained graphene bismaleimide resin composite material by S5.
7. the preparation method of graphene bismaleimide resin composite material according to claim 6, it is characterised in that: the step
S1 is specially that the mixed acid of the concentrated sulfuric acid and concentrated nitric acid is used to be surface-treated graphene, so that its surface is generated functional group, washes
Wash it is dry after mix with diallyl bisphenol and its homologue or aromatic amine, wherein graphene accounts for diallyl bisphenol and its together
The mass percent for being object or aromatic amine is 0.001%~3%, and stirring mixture makes it be uniformly dispersed, at 120 DEG C~180 DEG C
It is reacted 2 hours~6 hours under environment, reacts diallyl bisphenol and its homologue or aromatic amine groups sufficiently, two obtained
Allyl bisphenol-A graphene mixture is modified graphene.
8. a kind of preparation method of graphene bismaleimide resin composite material according to claim 7, it is characterised in that: described
It is 1:1~9 that the concentrated sulfuric acid, which accounts for the volume ratio of concentrated nitric acid, in mixed acid.
9. the preparation method of graphene bismaleimide resin composite material according to claim 6, it is characterised in that: the step
In S2, the molar ratio of allyl group and dimaleoyl imino group is 1:1~1.2, the toughener in modified graphene
For at least one of polysulfones, polyether sulfone, polyether sulphone, polyether-ether-ketone, poly(aryl ether ketone), polyimides or polyetherimide, increase
Tough dose accounts for the 1%~30% of graphene bismaleimide resin gross mass.
10. the preparation method of graphene bismaleimide resin composite material according to claim 6, it is characterised in that: the step
In rapid S4, graphene bismaleimide resin prepreg is flattened with electric iron, and the prepreg of paving uses and vacuumizes carry out pre-compacted.
11. the preparation method of graphene bismaleimide resin composite material according to claim 6, it is characterised in that: the step
Curing mode includes autoclave, press, baking oven in rapid S5.
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| CN110078952A (en) * | 2019-03-20 | 2019-08-02 | 青岛中维新材料有限公司 | A kind of preparation method of aramid fiber carbon fiber composite reinforced material |
| CN111040163A (en) * | 2019-11-29 | 2020-04-21 | 航天特种材料及工艺技术研究所 | Bismaleimide resin, air bag for autoclave molding and preparation method thereof |
| CN113072795A (en) * | 2021-03-15 | 2021-07-06 | 浙江宝旌炭材料有限公司 | Aramid fiber/graphene composite reinforced carbon fiber resin prepreg |
| CN114685990A (en) * | 2020-12-31 | 2022-07-01 | 洛阳尖端技术研究院 | Modified graphene/bismaleimide resin and preparation method thereof |
| CN116178954A (en) * | 2022-12-15 | 2023-05-30 | 常州天启新新科技有限公司 | Bismaleimide resin composite material for carbon fiber prepreg tape and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078952A (en) * | 2019-03-20 | 2019-08-02 | 青岛中维新材料有限公司 | A kind of preparation method of aramid fiber carbon fiber composite reinforced material |
| CN111040163A (en) * | 2019-11-29 | 2020-04-21 | 航天特种材料及工艺技术研究所 | Bismaleimide resin, air bag for autoclave molding and preparation method thereof |
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| CN113072795A (en) * | 2021-03-15 | 2021-07-06 | 浙江宝旌炭材料有限公司 | Aramid fiber/graphene composite reinforced carbon fiber resin prepreg |
| CN116178954A (en) * | 2022-12-15 | 2023-05-30 | 常州天启新新科技有限公司 | Bismaleimide resin composite material for carbon fiber prepreg tape and preparation method thereof |
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