CN115449110B - Aramid fiber reinforced epoxy resin matrix composite material and preparation method thereof - Google Patents
Aramid fiber reinforced epoxy resin matrix composite material and preparation method thereof Download PDFInfo
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- 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
- C08J5/246—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using polymer based synthetic fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/30—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core
- B29C70/34—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation
- B29C70/342—Shaping by lay-up, i.e. applying fibres, tape or broadsheet on a mould, former or core; Shaping by spray-up, i.e. spraying of fibres on a mould, former or core and shaping or impregnating by compression, i.e. combined with compressing after the lay-up operation using isostatic pressure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
- C08G59/502—Polyalkylene polyamines
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- 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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
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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
- C08J2363/02—Polyglycidyl ethers of bis-phenols
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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
- C08J2463/00—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
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/40—Weight reduction
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Abstract
The invention belongs to the technical field of preparation of fiber composite materials, and particularly relates to an aramid fiber reinforced epoxy resin matrix composite material and a preparation method thereof. The invention provides a preparation method of an aramid fiber reinforced epoxy resin matrix composite material, which comprises the following steps: mixing aramid-based epoxy resin, non-aramid-based epoxy resin, a diluent and an amine curing agent to obtain a modified epoxy resin system; coating the modified epoxy resin system on an aramid fiber product to obtain a prepreg; and laminating the prepregs, and performing vacuum auxiliary molding to obtain the aramid fiber reinforced epoxy resin matrix composite. The preparation method provided by the invention can realize normal-temperature curing of the epoxy resin composite material, and the prepared composite material has higher interfacial binding force.
Description
Technical Field
The invention belongs to the technical field of preparation of fiber composite materials, and particularly relates to an aramid fiber reinforced epoxy resin matrix composite material and a preparation method thereof.
Background
The aramid fiber has excellent performances of high strength, high modulus, high temperature resistance, flame retardance and the like, and the resin-based composite material taking the aramid fiber as a reinforcement is widely applied to the fields of national defense, airplanes, aerospace composite materials and the like. However, the surface of the aramid fiber presents inertia, so that the interfacial binding force between the aramid fiber and the resin is poor, and the application of the resin-based composite material is limited.
The molding process of the resin-based composite material is the development foundation and condition of the composite material industry. At present, more than 20 resin matrix composite material forming methods exist. Common processes include hand lay-up molding, spray molding, filament winding molding, compression molding, etc., but the above processes all require a high curing temperature (100 to 150 ℃) although they can produce a composite material with high adhesion of aramid fibers to resin.
Disclosure of Invention
In view of the above, the invention aims to provide an aramid fiber reinforced epoxy resin matrix composite material and a preparation method thereof. The preparation method provided by the invention can realize the normal-temperature solidification of the epoxy resin aramid fiber composite material, and the prepared aramid fiber reinforced epoxy resin matrix composite material has higher interfacial binding force.
In order to solve the problems, the invention provides a preparation method of an aramid fiber reinforced epoxy resin matrix composite material, which comprises the following steps:
mixing aramid-based epoxy resin, non-aramid-based epoxy resin, a diluent and an amine curing agent to obtain a modified epoxy resin system;
coating the modified epoxy resin system on an aramid fiber product to obtain a prepreg;
after laminating the prepregs, carrying out vacuum auxiliary forming to obtain the aramid fiber reinforced epoxy resin matrix composite; the vacuum auxiliary forming comprises vacuumizing and curing which are sequentially carried out; the curing temperature is 20-30 ℃.
Preferably, the vacuumizing pressure is-0.09 to-0.10 MPa, and the vacuumizing time is 5-10 min.
Preferably, the curing time is 6 to 7 hours.
Preferably, the number of layers of the prepreg is 6-12; the thickness of each layer of the prepreg is 0.12-0.16 mm.
Preferably, the mass ratio of the modified epoxy resin system to the aramid fiber product is 10-40: 100.
preferably, the amine curing agent comprises diethylenetriamine and/or triethylenetetramine.
Preferably, the diluent comprises one or more of butyl glycidyl ether, benzyl glycidyl ether, octyl glycidyl ether, 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, neopentyl glycol diglycidyl ether and trimethylolpropane triglycidyl ether.
Preferably, the non-aramid-based epoxy resin includes one or more of bisphenol a type epoxy resin, glycidylamine type and glycidylester type epoxy resin.
Preferably, the mass ratio of the aramid-based epoxy resin to the non-aramid-based epoxy resin is 1-6: 15-30; the mass ratio of the aramid-based epoxy resin to the amine curing agent is 1-6: 10 to 17; the mass ratio of the aramid-based epoxy resin to the diluent is 1-6: 1 to 3.
The invention also provides the aramid fiber reinforced epoxy resin matrix composite material prepared by the preparation method, and the interlayer shear strength of the aramid fiber reinforced epoxy resin matrix composite material is 30-35 MPa.
The invention provides a preparation method of an aramid fiber reinforced epoxy resin matrix composite material, which comprises the following steps: mixing aramid-based epoxy resin, non-aramid-based epoxy resin, a diluent and an amine curing agent to obtain a modified epoxy resin system; coating the modified epoxy resin system on an aramid fiber product to obtain a prepreg; after laminating the prepregs, carrying out vacuum auxiliary forming to obtain the aramid fiber reinforced epoxy resin matrix composite; the vacuum auxiliary forming comprises vacuumizing and curing which are sequentially carried out; the curing temperature is 20-30 ℃. The preparation method limits the raw material types of the aramid fiber reinforced epoxy resin matrix composite material, realizes the curing of the composite material by using an amine curing agent, and can realize the normal-temperature curing of the epoxy resin composite material by matching with a vacuum auxiliary process; meanwhile, the low-viscosity aramid-based epoxy resin which reserves an aramid skeleton is introduced, so that the cohesiveness of a resin matrix and aramid fibers is remarkably improved, and the interfacial cohesiveness between the aramid fibers and the resin matrix is improved.
Drawings
FIG. 1 is an SEM scanning image of a cured product of the modified epoxy resin system of example 1 and comparative example 1;
FIG. 2 SEM images of fracture surfaces of the composite materials prepared in example 1 and comparative example 1.
Detailed Description
The invention provides a preparation method of an aramid fiber reinforced epoxy resin matrix composite material, which comprises the following steps:
mixing aramid-based epoxy resin, non-aramid-based epoxy resin, a diluent and an amine curing agent to obtain a modified epoxy resin system;
coating the modified epoxy resin system on an aramid fiber product to obtain a prepreg;
after laminating the prepregs, carrying out vacuum auxiliary forming to obtain the aramid fiber reinforced epoxy resin matrix composite; the vacuum auxiliary forming comprises vacuumizing and curing which are sequentially carried out; the curing temperature is 20-30 ℃.
According to the invention, the modified epoxy resin system is obtained by mixing the aramid-based epoxy resin, the non-aramid-based epoxy resin, the diluent and the amine curing agent.
In the present invention, the preparation of the aramid-based epoxy resin preferably includes the steps of:
mixing aramid powder, ethylene oxide and epichlorohydrin, and carrying out grafting reaction under the catalysis of metal alkoxide to obtain the aramid-based epoxy resin.
In the invention, the aramid powder preferably comprises para-aramid or high-molecular defective aramid powder generated in the production process of para-aramid, and the molecular weight of the aramid is preferably 8000-14000. In the present invention, the metal alkoxide is preferably sodium methoxide; the mass ratio of the sodium methoxide to the ethylene oxide to the epichlorohydrin to the aramid powder is preferably 0.6-0.7: 2.5 to 2.6:2.0:1.0; more preferably 0.67:2.58:2.0:1. In the present invention, the temperature of the grafting reaction is preferably 100 to 130 ℃, more preferably 110 to 120 ℃, and the holding time is preferably 1.5 to 3.5 hours, more preferably 2 to 2.5 hours.
In the present invention, the viscosity of the aramid-based epoxy resin is preferably 350 to 600mpa·s; the epoxy value of the aramid-based epoxy resin is preferably 0.9 to 1.2eq/100g.
In the present invention, the non-aramid based epoxy resin preferably includes one or more of bisphenol a type epoxy resin, glycidylamine type and glycidylester type epoxy resin, more preferably bisphenol a type epoxy resin; the bisphenol A type epoxy resin is preferably E-51 epoxy resin. In an embodiment of the present invention, the E-51 epoxy resin is preferably provided by Anhui New technology Co., ltd.
In the present invention, the amine curing agent preferably includes diethylenetriamine and/or triethylenetetramine, more preferably triethylenetetramine. In the embodiment of the invention, the triethylene tetramine is preferably provided by Anhui Xinyun technology limited company.
In the present invention, the diluent preferably includes one or more of butyl glycidyl ether, benzyl glycidyl ether, octyl glycidyl ether, 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, neopentyl glycol diglycidyl ether, trimethylolpropane triglycidyl ether, and more preferably butyl glycidyl ether.
In the invention, the mass ratio of the aramid-based epoxy resin to the non-aramid-based epoxy resin is preferably 1-6: 15 to 30, more preferably 2 to 4:20 to 25. In the invention, the mass ratio of the aramid-based epoxy resin to the amine curing agent is preferably 1-6: 10 to 17, more preferably 2 to 4:13 to 14. In the invention, the mass ratio of the aramid-based epoxy resin to the diluent is preferably 1-6: 1 to 3, more preferably 2 to 4:1.5 to 2.5.
After the modified epoxy resin system is obtained, the modified epoxy resin system is coated on an aramid fiber product to obtain the prepreg.
In the present invention, the aramid fiber product preferably includes an aramid fiber cloth or an aramid fiber felt, and the aramid fiber cloth is preferably an aramid fiber cloth of a plain weave. In an embodiment of the present invention, the aramid fiber cloth is preferably provided by ceremonies chemical fiber stock, inc.
In the invention, the mass ratio of the modified epoxy resin system to the aramid fiber product in the prepreg is preferably 10-40: 100, more preferably 20 to 30:100.
after the prepreg is obtained, the aramid fiber reinforced epoxy resin matrix composite is obtained by laminating the prepreg and then performing vacuum auxiliary molding.
In the present invention, the number of layers of the prepreg is preferably 6 to 12, more preferably 8 to 10, and the thickness of each layer of the prepreg is preferably 0.12 to 0.16mm, more preferably 0.15mm.
In the invention, the vacuum-assisted molding comprises vacuum-pumping and curing which are sequentially carried out. In the present invention, the vacuum pressure is preferably-0.09 to-0.10 MPa, more preferably-0.09 MPa, and the time is preferably 5 to 10min, more preferably 6 to 7min.
In the present invention, the curing temperature is preferably 20 to 30 ℃, more preferably 25 ℃; the curing time is preferably 6 to 7 hours, more preferably 6.5 hours.
The invention also provides the aramid fiber reinforced epoxy resin-based composite material prepared by the preparation method, and the interlayer shear strength of the aramid fiber reinforced epoxy resin/aramid fiber composite material is preferably 30-35 MPa.
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
67g of aramid powder (molecular weight is 12000), 258g of ethylene oxide and 200g of epichlorohydrin are mixed, and grafting reaction is carried out under the catalysis of 100g of metal alkoxide (reaction temperature is 130 ℃ C., time is 2.5 h), so that the aramid-based epoxy resin is obtained.
100g E-51 epoxy resin, 3g butyl glycidyl ether and 2.5% of aramid-based epoxy resin added to E-51 epoxy mass fraction are stirred and mixed uniformly, and then 13.6g triethylene tetramine is added and mixed uniformly, so that a modified epoxy resin system is obtained.
Uniformly coating the obtained modified epoxy resin system on aramid fiber cloth to obtain prepreg (the mass ratio of the modified epoxy resin system to the aramid fiber cloth in the prepreg is 20:100), laminating 8 layers of prepreg, wherein the size of each layer of aramid fiber cloth is 80cm, the thickness of each layer is 0.15mm, carrying out vacuum auxiliary forming on the laminated prepreg, and carrying out vacuum auxiliary forming sequentially, namely vacuumizing (the pressure is-0.09 MPa, the time is 5 min) and curing (the temperature is 25 ℃ and the time is 6 h) to obtain the aramid fiber reinforced epoxy resin matrix composite material.
Example 2
67g of aramid powder (molecular weight is 12000), 258g of ethylene oxide and 200g of epichlorohydrin are mixed, and grafting reaction is carried out under the catalysis of 100g of metal alkoxide (reaction temperature is 130 ℃ C., time is 2.5 h), so that the aramid-based epoxy resin is obtained.
100g E-51 epoxy resin, 3g butyl glycidyl ether and 5% of aramid-based epoxy resin added to E-51 epoxy mass fraction are stirred and mixed uniformly, and then 14.2g triethylene tetramine is added and mixed uniformly, so that a modified epoxy resin system is obtained.
Uniformly coating the obtained modified epoxy resin system on aramid fiber cloth to obtain prepreg (the mass ratio of the modified epoxy resin system to the aramid fiber cloth in the prepreg is 20:100), laminating 8 layers of prepreg, wherein the size of each layer of aramid fiber cloth is 80cm, the thickness of each layer is 0.15mm, carrying out vacuum auxiliary forming on the laminated prepreg, and carrying out vacuum auxiliary forming sequentially, namely vacuumizing (the pressure is-0.09 MPa, the time is 5 min) and curing (the temperature is 25 ℃ and the time is 6 h) to obtain the aramid fiber reinforced epoxy resin matrix composite material.
Example 3
67g of aramid powder (molecular weight is 12000), 258g of ethylene oxide and 200g of epichlorohydrin are mixed, and grafting reaction is carried out under the catalysis of 100g of metal alkoxide (reaction temperature is 130 ℃ C., time is 2.5 h), so that the aramid-based epoxy resin is obtained.
100g E-51 epoxy resin, 3g butyl glycidyl ether and 7.5% of aramid-based epoxy resin added to E-51 epoxy mass fraction are stirred and mixed uniformly, and then 14.7g triethylene tetramine is added and mixed uniformly, so that a modified epoxy resin system is obtained.
Uniformly coating the obtained modified epoxy resin system on aramid fiber cloth to obtain prepreg (the mass ratio of the modified epoxy resin system to the aramid fiber cloth in the prepreg is 20:100), laminating 8 layers of prepreg, wherein the size of each layer of aramid fiber cloth is 80cm, the thickness of each layer is 0.15mm, carrying out vacuum auxiliary forming on the laminated prepreg, and carrying out vacuum auxiliary forming sequentially, namely vacuumizing (the pressure is-0.09 MPa, the time is 5 min) and curing (the temperature is 25 ℃ and the time is 6 h) to obtain the aramid fiber reinforced epoxy resin matrix composite material.
Comparative example 1
100g E-51 epoxy resin, 3g butyl glycidyl ether and 0% of aramid-based epoxy resin added to E-51 epoxy mass fraction are stirred and mixed uniformly, and then 13.0g triethylene tetramine is added and mixed uniformly, so that a modified epoxy resin system is obtained.
Uniformly coating the obtained modified epoxy resin system on aramid fiber cloth to obtain prepreg (the mass ratio of the modified epoxy resin system to the aramid fiber cloth in the prepreg is 20:100), laminating 8 layers of prepreg, wherein the size of each layer of aramid fiber cloth is 80cm, the thickness of each layer is 0.15mm, carrying out vacuum auxiliary forming on the laminated prepreg, and carrying out vacuum auxiliary forming sequentially, namely vacuumizing (the pressure is-0.09 MPa, the time is 5 min) and curing (the temperature is 25 ℃ and the time is 6 h) to obtain the aramid fiber reinforced epoxy resin matrix composite material.
Test case
1. Mechanical properties of epoxy resin cured product
(1) Example 1 mechanical Properties of epoxy resin cured product
The modified epoxy resin systems prepared in examples 1-3 and comparative example 1 are poured into a mold, then placed in a vacuum drying oven, vacuumized for 5min (the pressure is-0.09 MPa), cured for 6h at normal temperature, and the epoxy resin cured product is obtained after demolding. The invention tests the performance of the epoxy resin condensate, and the testing method comprises the following steps: tensile strength was tested according to GB/T2567-2008 using type II samples; impact strength was measured according to GB/T2567-2008 using a notched specimen with dimensions of 4mm 10mm 80mm; the bending strength was measured according to GB/T2567-2008, and the mechanical properties were measured as shown in Table 1.
TABLE 1 mechanical Properties of epoxy resin cured product of example 1
As can be seen from table 1: at an aramid-based epoxy resin incorporation level of 2.5wt.%, the epoxy resin cured product reached maximum values of 66.25MPa and 15.60KJ/m in tensile strength and impact strength 2 The elongation at break also reaches 2.76%, the bending strength reaches 99.52MPa, and the performances are improved.
(2) SEM electron microscope scanning analysis of epoxy resin cured product
In the invention, after gold plating is carried out on the cross-section surfaces of the epoxy resin cured products of the example 1 and the comparative example 1, SEM scanning is carried out, the scanning image is shown in figure 1, wherein figure 1 (a) is a scanning electron microscope image of the epoxy resin cured product obtained in the comparative example 1; fig. 1 (b) is a scanning electron microscope image of the cured epoxy resin obtained in example 1, and it can be seen from fig. 1: the fracture surface of the epoxy resin cured product added with the aramid-based epoxy resin has more microcracks. When external impact is applied, microcracks spread around and absorb energy, so that the impact strength is improved, and the toughness fracture is realized.
2. Interlaminar shear Strength test
The invention tests interlayer shear strength of the aramid fiber reinforced epoxy resin matrix composite materials prepared in the example 1, the example 3 and the comparative example 1, and tests the dimension pieces of the sample bars in table 2, the test method: the test was performed by a universal tester at a test speed of 1.0mm/min according to ASTM D2 344. The composite materials of different aramid-based epoxy resins were tested for 5 samples, respectively, and the average value of the obtained results was used as the interlaminar shear strength, and the test results are shown in table 2, respectively.
TABLE 2 interlaminar shear Strength of composite materials prepared in example 1
As can be seen from Table 2, the aramid-based epoxy resin effectively improves the interfacial bonding performance of the aramid fiber and the E-51 resin, the interlayer shear strength of the composite material can reach about 34.42MPa, and the shear strength of the composite material is improved by 12% compared with that of the composite material without the aramid-based epoxy resin, which indicates that the curing of the aramid-based epoxy resin modified composite material under normal temperature conditions can effectively improve the interfacial performance between the aramid fiber and the epoxy resin.
3. Flexural Strength test
The invention tests interlayer shear strength of the aramid fiber reinforced epoxy resin matrix composite materials prepared in the example 1, the example 3 and the comparative example 1, and tests the dimension piece of the sample bar, table 3, test method: the test was performed by a universal tester at a test speed of 1.0mm/min according to ASTM D7 264 standard. The composite materials of different aramid-based epoxy resins were tested for 5 samples, respectively, and the average value of the results was obtained as bending strength. The test results are shown in Table 3, respectively.
TABLE 3 flexural Strength and interlaminar shear Strength of composite materials
As can be seen from Table 3, the bending performance of the composite material added with the aramid-based epoxy resin is improved, and the aramid-based epoxy resin contains more complete aramid molecular chains, and the amide bond of the aramid-based epoxy resin is grafted with an ethoxy chain with flexibility, so that a longer flexible chain can be effectively formed to bear bending load, and the bending performance of the composite material can be improved. When the addition amount of the aramid-based epoxy resin is 2.5 wt%, the bending strength of the composite material reaches the maximum 313.22MPa, and is improved by 5% compared with the composite material without the aramid-based epoxy resin.
4. Fracture SEM analysis
After gold plating is carried out on the surface of the fracture surface of the composite material prepared in the embodiment 1 and the comparative example 1, SEM scanning is carried out by using an environmental scanning electron microscope of the type Quanta 200 in the United states, the SEM scanning electron microscope is shown in figure 2, wherein figure 2 (i) is the fracture surface of the composite material of the comparative example 1; FIG. 2 (j) shows the fracture surface of the composite material of example 1. As is clear from (i) and (j), the composite material added with the aramid-based epoxy resin has more fiber surface particles, the surface of the aramid fiber is not damaged, and the density among the fibers is high. The structural advantage of the aramid-based epoxy resin can be exerted under the normal-temperature curing condition.
The foregoing is merely illustrative of the preferred embodiments of this invention, and it will be appreciated by those skilled in the art that variations and modifications may be made without departing from the principles of the invention, and such variations and modifications are to be regarded as being within the scope of the invention.
Claims (10)
1. The preparation method of the aramid fiber reinforced epoxy resin matrix composite material is characterized by comprising the following steps of:
mixing aramid-based epoxy resin, non-aramid-based epoxy resin, a diluent and an amine curing agent to obtain a modified epoxy resin system;
coating the modified epoxy resin system on an aramid fiber product to obtain a prepreg;
after laminating the prepregs, carrying out vacuum auxiliary forming to obtain the aramid fiber reinforced epoxy resin matrix composite; the vacuum auxiliary forming comprises vacuumizing and curing which are sequentially carried out; the curing temperature is 20-30 ℃.
2. The preparation method according to claim 1, wherein the vacuum pressure is-0.09 to-0.10 MPa for 5 to 10min.
3. The method of claim 1, wherein the curing time is from 6 to 7 hours.
4. The method of claim 1, wherein the number of layers of the prepreg is 6 to 12; the thickness of each layer of the prepreg is 0.12-0.16 mm.
5. The preparation method according to claim 1, wherein the mass ratio of the modified epoxy resin system to the aramid fiber product is 10-40: 100.
6. the method of claim 1, wherein the amine curing agent comprises diethylenetriamine and/or triethylenetetramine.
7. The preparation method according to claim 1, wherein the diluent comprises one or more of butyl glycidyl ether, benzyl glycidyl ether, octyl glycidyl ether, 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, neopentyl glycol diglycidyl ether and trimethylolpropane triglycidyl ether.
8. The method of claim 1, wherein the non-aramid based epoxy resin comprises one or more of bisphenol a type epoxy resin, glycidylamine type and glycidylester type epoxy resin.
9. The preparation method according to claim 1, wherein the mass ratio of the aramid-based epoxy resin to the non-aramid-based epoxy resin is 1-6: 15-30; the mass ratio of the aramid-based epoxy resin to the amine curing agent is 1-6: 10 to 17; the mass ratio of the aramid-based epoxy resin to the diluent is 1-6: 1 to 3.
10. The aramid fiber reinforced epoxy resin-based composite material prepared by the preparation method of any one of claims 1 to 9, which is characterized in that the interlaminar shear strength of the aramid fiber reinforced epoxy resin-based composite material is 30 to 35MPa.
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| CN107674222A (en) * | 2017-11-02 | 2018-02-09 | 北京化工大学 | A kind of aramid fiber composite material preparation method of interfacial adhesion enhancing |
| CN108047429A (en) * | 2017-12-15 | 2018-05-18 | 南京林业大学 | A kind of aramid fiber base epoxy and preparation method thereof |
| CN109486454A (en) * | 2017-09-09 | 2019-03-19 | 熊小利 | A kind of room temperature curing toughened epoxy resin adhesive and preparation method thereof |
| CN109680496A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | Aramid fiber surface modifying method and surface modifying aramid fiber |
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| CN109486454A (en) * | 2017-09-09 | 2019-03-19 | 熊小利 | A kind of room temperature curing toughened epoxy resin adhesive and preparation method thereof |
| CN109680496A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | Aramid fiber surface modifying method and surface modifying aramid fiber |
| CN107674222A (en) * | 2017-11-02 | 2018-02-09 | 北京化工大学 | A kind of aramid fiber composite material preparation method of interfacial adhesion enhancing |
| CN108047429A (en) * | 2017-12-15 | 2018-05-18 | 南京林业大学 | A kind of aramid fiber base epoxy and preparation method thereof |
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