CN109206905B - Graphene bismaleimide resin composite material and preparation method thereof - Google Patents
Graphene bismaleimide resin composite material and preparation method thereof Download PDFInfo
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- 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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- 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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- 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
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Abstract
The invention relates to a graphene bismaleimide resin composite material. The graphene bismaleimide resin prepreg is formed by laminating and co-curing a plurality of layers of graphene bismaleimide resin prepreg layers and reinforcing materials consisting of carbon fibers, quartz fibers, glass fibers, aramid fibers and fabrics thereof. The obtained graphene bismaleimide resin composite material has the characteristics of light weight, high temperature resistance, good mechanical property, good electric and thermal conductivity and the like, and has wide application in the fields of aerospace, electronic information and high and new technology.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a graphene bismaleimide resin composite material and a preparation method thereof.
Background
The Bismaleimide (BMI) is a bifunctional compound taking maleimide as an active end group, can be copolymerized with various compounds to modify the bifunctional compound into a tough heat-resistant resin, and has a main chain containing an aromatic ring and a nitrogen heterocyclic structure, so that the resin has various excellent properties of high temperature resistance, humidity and heat resistance, radiation resistance, high insulation, friction resistance, flame retardance, good mechanical property, good dimensional stability and the like, and is widely applied to the fields of national defense, aerospace, electronics and the like. As a novel nano material, compared with materials such as carbon nanotubes and the like, the graphene has a stable lattice structure and extremely high current carriers, and has extremely good electrical conductivity and thermal conductivity. At present, a graphene material is mainly used as a filler to be mixed with other components, the electrical property, the thermal property and other properties of the material are improved, a main method is to disperse graphene in other materials to prepare a composite material, the scheme is difficult to solve the dispersion problem of graphene, the graphene is easy to damage by using a mechanical method, the interface property of the graphene and a matrix is poor, a solution dispersion method is adopted, only a wet prepreg can be prepared, the purposes of high heat and electrical conductivity and good comprehensive mechanical property cannot be achieved at the same time, the actual requirement is difficult to meet, and the wide application of the graphene material is limited.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the graphene bismaleimide resin composite material and the preparation method thereof, and the graphene bismaleimide resin composite material has the characteristics of light weight, high temperature resistance, good mechanical property, good electric conductivity and thermal conductivity and the like.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a graphene bismaleimide resin composite material is characterized in that a plurality of layers of graphene bismaleimide resin and fiber composite prepregs are alternately stacked and distributed in the graphene bismaleimide resin composite material, the modified graphene in the graphene bismaleimide resin is uniformly distributed in bismaleimide monomers, the surface of the graphene is treated by adopting mixed acid of concentrated sulfuric acid and concentrated nitric acid to generate functional groups on the surface of the graphene, the graphene is mixed with diallyl bisphenol A or diallyl bisphenol A and aromatic amine after being washed and dried, wherein the graphene accounts for 0.001-3% of the mass of the diallyl bisphenol A or the diallyl bisphenol A and the aromatic amine, the mixture is stirred to be uniformly dispersed, and reacting for 2-6 hours at 120-180 ℃ to ensure that diallyl bisphenol A or diallyl bisphenol A and aromatic amine groups are fully reacted to obtain a diallyl bisphenol A graphene mixture, namely the modified graphene.
Preferably, the fiber is at least one selected from the group consisting of carbon fiber, quartz fiber, glass fiber, aramid fiber, and woven fabric of the foregoing fibers.
Preferably, the molar ratio of allyl groups to bismaleimide groups in the graphene bismaleimide resin is 1: 1-1.2.
Preferably, the graphene is 0.001 to 3% by mass of the bismaleimide resin.
Preferably, the resin content of the prepreg compounded by the graphene bismaleimide resin and the fibers is 25-60%, and the single-layer curing thickness is 0.01-0.45 mm.
The preparation method of the graphene bismaleimide resin composite material comprises the following steps:
s1, preparing modified graphene; carrying out surface treatment on graphene by using mixed acid of concentrated sulfuric acid and concentrated nitric acid to enable the surface of the graphene to generate functional groups, washing, drying, mixing with diallyl bisphenol A or diallyl bisphenol A and aromatic amine, wherein the mass percent of the graphene in the diallyl bisphenol A or the diallyl bisphenol A and the aromatic amine is 0.001% -3%, stirring the mixture to uniformly disperse, reacting for 2-6 hours at 120-180 ℃, and enabling the diallyl bisphenol A or the diallyl bisphenol A to fully react with the aromatic amine groups to obtain a diallyl bisphenol A graphene mixture, namely modified graphene.
S2, preparing graphene bismaleimide resin, and fully mixing and dispersing the modified graphene, bismaleimide monomer, modifier and toughening agent to prepare the graphene bismaleimide resin;
s3, preparing graphene bismaleimide resin into a glue film on a glue film machine according to the resin content requirement and the surface density of the fiber reinforced material, and compounding the glue film with carbon fibers, quartz fibers, glass fibers, aramid fibers and fabrics of the carbon fibers, the quartz fibers, the glass fibers and the aramid fibers on a compounding machine to prepare graphene bismaleimide resin prepreg; wherein the thickness of the adhesive film is calculated according to the resin content and the reinforced material;
s4, cutting the graphene bismaleimide resin prepreg according to the size of the die; laminating and paving the cut graphene bismaleimide resin prepreg on a die to obtain a composite material blank;
and S5, curing the laid composite material blank to obtain the graphene bismaleimide resin composite material.
Preferably, the volume ratio of the concentrated sulfuric acid in the mixed acid to the concentrated nitric acid is 1: 1-9.
Preferably, in step S2, the molar ratio of allyl groups to bismaleimide groups in the modified graphene is 1: 1-1.2, the toughening agent is at least one of polysulfone, polyethersulfone, polyetheretherketone, polyaryletherketone, and polyimide, and the toughening agent accounts for 1% -30% of the total mass of the graphene bismaleimide resin.
Preferably, in step S4, the graphene bismaleimide resin prepreg is flattened by an electric iron, and the laid prepreg is pre-compacted by vacuum pumping.
Preferably, the curing manner in step S5 includes autoclave, press, and oven.
After the technical scheme is adopted, the invention has the following technical effects:
the composite material provided by the invention adopts a composite scheme of graphene bismaleimide resin and a reinforced fiber layer, so that the material has good electric and heat conducting properties. In addition, the composite material adopts the reinforced fibers, and the reinforced fibers have small specific gravity, large specific strength and large specific modulus. The composite material obtains comprehensive properties which cannot be achieved by a single composition material through complementation and correlation of properties of all components, has small specific gravity and large specific strength and specific modulus, solves the problems of determination of large specific gravity, small specific strength and the like of the existing graphene composite material, and obviously improves the mechanical properties of the material. The surface resistance of the graphene bismaleimide composite material is less than 50 omega, the bending strength of the graphene bismaleimide composite material and a T700-grade carbon fiber composite material is greater than 1400MPa, the interlaminar shear strength is greater than 75MPa, the tensile strength is greater than 1700MPa, and the 0-degree compression strength is greater than 1050 MPa.
Detailed Description
The graphene bismaleimide resin composite material and the preparation method thereof according to the present invention are further described below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1:
the preparation method of the graphene bismaleimide resin composite material containing 8 layers of graphene bismaleimide resin prepreg comprises the following steps:
(1) preparation of graphene bismaleimide resin T700 fiber unidirectional prepreg
(a) Preparation of modified graphene
Dispersing graphene in mixed acid (volume ratio is 1:1) of concentrated sulfuric acid and concentrated nitric acid, and carrying out ultrasonic reaction for 48h at normal temperature; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, the filtrate was washed to neutrality and dried. Mixing the treated graphene with 99% of diallyl bisphenol A according to the mass ratio of 1%, uniformly dispersing the graphene by adopting a high-speed stirring method, and reacting for 4 hours at 150 ℃ to fully react the diallyl bisphenol A with the surface groups of the graphene to obtain a diallyl bisphenol A graphene mixture;
(b) preparation of graphene bismaleimide resin
Mixing a diallyl bisphenol A graphene mixture with a bismaleimide monomer, a toughening agent and a modifier, wherein the molar ratio of allyl groups to bismaleimide groups is 1:1, the toughening agent is polyarylethersulfone, and the toughening agent is 15% of the total mass ratio, and mixing on equipment to prepare graphene bismaleimide resin;
(c) preparing graphene bismaleimide resin into an adhesive film, and compounding the adhesive film with quartz fiber fabric to form graphene bismaleimide resin prepreg, wherein the content of the prepreg resin is 35%, and the fiber areal density is 133g/m2The monolayer thickness after curing was 0.125 mm.
(2) Cutting the graphene bismaleimide resin prepreg according to the size of a mould, paving and pasting 8 layers of the graphene bismaleimide resin prepreg on the mould, allowing the prepreg to be flattened by an electric iron, allowing the prepreg to be pre-compacted by vacuumizing according to the process requirement, and curing the paved composite material blank by adopting an autoclave, a press, an oven or other modes according to the curing system of the graphene bismaleimide resin composite material.
(3) And demolding to obtain the graphene bismaleimide resin composite material.
The surface resistance of the graphene bismaleimide resin T700 composite material is less than 50 omega, the bending strength is greater than 1400MPa, the interlaminar shear strength is greater than 75MPa, the tensile strength is greater than 1700MPa, and the 0-degree compressive strength is greater than 1050 MPa.
Example 2:
the preparation method of the graphene bismaleimide resin composite material containing 16 layers of graphene bismaleimide resin prepreg comprises the following steps:
(1) preparation of graphene bismaleimide resin glass fiber fabric prepreg
(a) Preparation of modified graphene
Dispersing graphene in mixed acid (volume ratio is 1:9) of concentrated sulfuric acid and concentrated nitric acid, and stripping at normal temperature for ultrasonic reaction for 48 hours; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, the filtrate was washed to neutrality and dried. Mixing the treated graphene with 97% of diallyl bisphenol A according to the mass ratio of 3%, uniformly dispersing the graphene by adopting a high-speed stirring method, and reacting for 4 hours at 150 ℃ to fully react the diallyl bisphenol A with the surface groups of the graphene to obtain a diallyl bisphenol A graphene mixture;
(b) preparation of graphene bismaleimide resin
Mixing a diallyl bisphenol A graphene mixture with a bismaleimide monomer, a toughening agent and a modifier, wherein the molar ratio of allyl groups to bismaleimide groups is 1:1.05, the toughening agent is polyarylethersulfone, and the toughening agent is 12% of the total mass ratio, and mixing on equipment to prepare graphene bismaleimide resin;
(c) preparing graphene bismaleimide resin into an adhesive film, and compounding the adhesive film with quartz fiber fabric to form graphene bismaleimide resin prepreg, wherein the content of the prepreg resin is 40%, and the fiber areal density is 295g/m2The monolayer thickness after curing was 0.28 mm.
(2) Cutting the graphene bismaleimide resin prepreg according to the size of a mould, paving and pasting 16 layers of the graphene bismaleimide resin prepreg on the mould, allowing the prepreg to be flattened by an electric iron, allowing the prepreg to be pre-compacted by vacuumizing according to the process requirement, and curing the paved composite material blank by adopting an autoclave, a press, an oven or other modes according to the curing system of the graphene bismaleimide resin composite material.
(3) And demolding to obtain the graphene bismaleimide resin composite material.
The surface resistance of the graphene bismaleimide glass fiber composite material is less than 50 omega, the bending strength is greater than 800MPa, the interlaminar shear strength is greater than 55MPa, the tensile strength is greater than 750MPa, and the 0-degree compressive strength is greater than 650 MPa.
Example 3:
the preparation method of the graphene bismaleimide resin composite material containing 4 layers of graphene bismaleimide resin prepreg comprises the following steps:
(1) preparation of graphene bismaleimide resin quartz fiber fabric prepreg
(a) Preparation of modified graphene
Dispersing graphene in mixed acid (volume ratio is 4:6) of concentrated sulfuric acid and concentrated nitric acid, and stripping at normal temperature for ultrasonic reaction for 48 hours; and after the ultrasonic treatment is finished, dropwise adding deionized water to dilute the concentrated acid solution, and continuously stirring while dropwise adding. After dilution, the filtrate was washed to neutrality and dried. Mixing the treated graphene with 93% of diallyl bisphenol A and 5% of diamino diphenyl sulfone according to the mass ratio of 2%, uniformly dispersing the graphene by adopting a high-speed stirring method, and reacting for 4 hours at 150 ℃ to fully react the diallyl bisphenol A, the diamino diphenyl sulfone and the surface groups of the graphene to obtain a graphene mixture;
(b) preparation of graphene bismaleimide resin
Mixing a diallyl bisphenol A graphene mixture with a bismaleimide monomer, a toughening agent and a modifier, wherein the molar ratio of allyl groups to bismaleimide groups is 1:1, the toughening agent is polyarylethersulfone, and the toughening agent is 17% of the total mass ratio, and mixing on equipment to prepare graphene bismaleimide resin;
(c) preparing graphene bismaleimide resin into an adhesive film, and compounding the adhesive film with quartz fiber fabric to form graphene bismaleimide resin prepreg, wherein the content of the prepreg resin is 40%, and the fiber areal density is 125g/m2The monolayer thickness after curing was 0.12 mm.
(2) Cutting the graphene bismaleimide resin prepreg according to the size of a mould, paving and pasting 16 layers of the graphene bismaleimide resin prepreg on the mould, allowing the prepreg to be flattened by an electric iron, allowing the prepreg to be pre-compacted by vacuumizing according to the process requirement, and curing the paved composite material blank by adopting an autoclave, a press, an oven or other modes according to the curing system of the graphene bismaleimide resin composite material.
(3) And demolding to obtain the graphene bismaleimide resin composite material.
The surface resistance of the graphene bismaleimide resin quartz composite material is less than 50 omega, the bending strength is greater than 750MPa, the interlaminar shear strength is greater than 55MPa, the tensile strength is greater than 650MPa, and the 0-degree compressive strength is greater than 600 MPa.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A graphene bismaleimide resin composite material is characterized in that: the modified graphene is uniformly distributed in a bismaleimide monomer, the surface of the modified graphene is treated by using mixed acid of concentrated sulfuric acid and concentrated nitric acid to enable the surface of the modified graphene to generate functional groups, the modified graphene is mixed with diallyl bisphenol A or diallyl bisphenol A and aromatic amine after being washed and dried, wherein the mass percentage of the graphene to the diallyl bisphenol A or the diallyl bisphenol A to the aromatic amine is 0.001% -3%, the mixture is stirred to be uniformly dispersed, the mixture is reacted for 2-6 hours at the temperature of 120-180 ℃, the diallyl bisphenol A or the diallyl bisphenol A and the aromatic amine are fully reacted, and the obtained diallyl bisphenol A graphene mixture is the modified graphene.
2. The graphene bismaleimide resin composite material of claim 1, wherein: the fiber is selected from at least one of carbon fiber, quartz fiber, glass fiber, aramid fiber and fabric of the fiber.
3. The graphene bismaleimide resin composite material of claim 1, wherein: the graphene bismaleimide resin comprises allyl groups and bismaleimide groups, wherein the molar ratio of the allyl groups to the bismaleimide groups in the graphene bismaleimide resin is 1: 1-1.2.
4. The graphene bismaleimide resin composite material of claim 1, wherein: the mass proportion of the graphene in the bismaleimide resin is 0.001% -3%.
5. The graphene bismaleimide resin composite material of claim 1, wherein: the resin content of the prepreg compounded by the graphene bismaleimide resin and the fiber is 25% -60%, and the single-layer curing thickness is 0.01 mm-0.45 mm.
6. The method for preparing a graphene bismaleimide resin composite material as claimed in any one of claims 1 to 5, comprising the steps of:
s1, preparing modified graphene, carrying out surface treatment on the graphene by adopting mixed acid of concentrated sulfuric acid and concentrated nitric acid to enable the surface of the graphene to generate functional groups, washing and drying the graphene, mixing the graphene with diallyl bisphenol A or diallyl bisphenol A and aromatic amine, wherein the mass percentage of the graphene in the diallyl bisphenol A or the diallyl bisphenol A and the aromatic amine is 0.001% -3%, stirring the mixture to enable the mixture to be uniformly dispersed, reacting for 2-6 hours at 120-180 ℃, and enabling the diallyl bisphenol A or the diallyl bisphenol A to fully react with the aromatic amine groups to obtain a diallyl bisphenol A graphene mixture, namely the modified graphene;
s2, preparing graphene bismaleimide resin, and fully mixing and dispersing the modified graphene, bismaleimide monomer, modifier and toughening agent to prepare the graphene bismaleimide resin;
s3, preparing graphene bismaleimide resin into a glue film on a glue film machine according to the resin content requirement and the surface density of the fiber reinforced material, and compounding the glue film with carbon fibers, quartz fibers, glass fibers, aramid fibers and fabrics of the carbon fibers, the quartz fibers, the glass fibers and the aramid fibers on a compounding machine to prepare graphene bismaleimide resin prepreg;
s4, cutting the graphene bismaleimide resin prepreg according to the size of the die; laminating and paving the cut graphene bismaleimide resin prepreg on a die to obtain a composite material blank;
and S5, curing the laid composite material blank to obtain the graphene bismaleimide resin composite material.
7. The preparation method of the graphene bismaleimide resin composite material as claimed in claim 6, wherein the graphene bismaleimide resin composite material comprises: the volume ratio of the concentrated sulfuric acid in the mixed acid to the concentrated nitric acid is 1: 1-9.
8. The method for preparing the graphene bismaleimide resin composite material as claimed in claim 6, wherein: in the step S2, the molar ratio of allyl groups to bismaleimide groups in the modified graphene is 1: 1-1.2, the toughening agent is at least one of polysulfone, polyethersulfone, polyetheretherketone, polyaryletherketone, and polyimide, and the toughening agent accounts for 1% -30% of the total mass of the graphene bismaleimide resin.
9. The method for preparing the graphene bismaleimide resin composite material as claimed in claim 6, wherein: in the step S4, the graphene bismaleimide resin prepreg is flattened by an electric iron, and the laid prepreg is pre-compacted by vacuum pumping.
10. The method for preparing the graphene bismaleimide resin composite material as claimed in claim 6, wherein: the curing mode in the step S5 comprises an autoclave, a press and an oven.
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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 |
| CN111040163B (en) * | 2019-11-29 | 2022-09-16 | 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 |
| 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 |
| 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 |
| CN116178954B (en) * | 2022-12-15 | 2023-10-03 | 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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