CN110372998B - 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 PDF

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CN110372998B
CN110372998B CN201910694442.3A CN201910694442A CN110372998B CN 110372998 B CN110372998 B CN 110372998B CN 201910694442 A CN201910694442 A CN 201910694442A CN 110372998 B CN110372998 B CN 110372998B
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epoxy resin
aramid fiber
composite material
fiber reinforced
matrix composite
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CN110372998A (en
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史振宇
崔鹏
王兆辉
袭建人
杨晓涛
张帅
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Shandong University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2477/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2477/10Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides
    • D06M2101/36Aromatic polyamides

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Abstract

The invention provides an aramid fiber reinforced epoxy resin matrix composite material and a preparation method thereof, wherein the preparation method comprises the steps of impregnating an aramid fiber fabric subjected to dopamine modification treatment with an epoxy resin curing agent solution to obtain a composite prepreg, and heating and pre-curing the composite prepreg after laminating and pressurizing the composite prepreg to obtain a pre-cured material; and (3) under the condition that the epoxy resin in the pre-cured material is in a semi-solid state, pouring an epoxy resin curing agent into the pre-cured material by using a vacuum pouring method to thicken the surface layer of the pre-cured material, and then carrying out secondary curing to obtain the epoxy resin curing agent. The invention changes the manufacturing process of the aramid fiber composite material plate to obtain good processability, thereby effectively solving the problem that the existing aramid fiber composite material processing technology is easy to generate processing defects and having good practical application value.

Description

Aramid fiber reinforced epoxy resin matrix composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to an aramid fiber reinforced epoxy resin matrix composite material and a preparation method thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the increasingly wide application of fiber reinforced composites in various industries, the fiber reinforced composites can be processed with high efficiency and high precision, and the further popularization and use of the fiber reinforced composites are limited. The composite material difficult to process represented by the aramid fiber composite material is a processing problem to be solved urgently in the current engineering problem. The inventors have found that due to the high strength and toughness of the fibres, the material exhibits mechanical anisotropy, and that defects commonly seen in processing include delamination, burrs and tears.
Meanwhile, the existing aramid fiber composite material plate is generally low in fiber content, the mass percentage is only 30% -40%, the thickness of a surface layer matrix of the plate is similar to that of an interlayer matrix, the extremely thin matrix cannot provide enough support for fibers in the machining process, the fibers are easy to break, the fibers are difficult to cut, and the machining quality is further deteriorated.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the aramid fiber reinforced epoxy resin matrix composite material and the preparation method thereof, and the aramid fiber reinforced epoxy resin matrix composite material has high fiber content and high surface layer matrix thickness by changing the manufacturing process of the aramid fiber composite material plate, so that the composite material has good mechanical property and processability (such as machinability), the problem that the processing defect is easy to generate in the existing aramid fiber composite material processing technology is effectively solved, and the processability of the material is improved.
The invention is realized by the following technical scheme:
the invention provides an aramid fiber reinforced epoxy resin matrix composite material, which comprises the following raw materials in parts by mass:
65-70 parts of modified aramid fiber, 30-35 parts of epoxy resin, 8-12 parts of curing agent, 1-2 parts of coupling agent and 0.5-1 part of antioxidant and ultraviolet absorbent.
The modified aramid fiber is dopamine modified aramid fiber, preferably, the modification treatment time is 2 hours, and the dopamine concentration is 2 g/L;
the curing agent is an epoxy resin curing agent, and is further preferably SH-200/201;
the coupling agent is: a silane coupling agent kh560 added only to the epoxy resin;
the antioxidant is as follows: V73-P; the ultraviolet absorbent is: UV-196, used in combination.
Preferably, the thickness of the surface matrix of the aramid fiber reinforced epoxy resin matrix composite material is not less than 250 μm; the thickness of the matrix between the aramid fiber fabric layers is not more than 10 mu m.
In a second aspect of the present invention, there is provided a method for preparing an aramid fiber-reinforced epoxy resin matrix composite material, the method comprising:
impregnating aramid fiber fabric subjected to dopamine modification treatment with an epoxy resin curing agent solution to obtain a composite prepreg, and heating and pre-curing the composite prepreg after laminating and pressurizing the composite prepreg to obtain a pre-cured material; and (3) under the condition that the epoxy resin in the pre-cured material is in a semi-solid state, pouring an epoxy resin curing agent into the pre-cured material by using a vacuum pouring method to thicken the surface layer of the pre-cured material, and then carrying out secondary curing to obtain the epoxy resin curing agent.
The preparation method of the dopamine modified aramid fiber fabric comprises the following steps: the aramid fiber fabric is soaked in the dopamine ethanol solution, and a layer of polydopamine coating is deposited on the surface of the aramid fiber by utilizing the oxidative autopolymerization of dopamine, so that the subsequent interfacial property of the aramid fiber/epoxy resin is effectively improved.
Further, the soaking temperature is controlled to be 45-55 ℃ (preferably 50 ℃), the soaking time is controlled to be 1.5-3 h (preferably 2h), and the concentration of dopamine is 1.8-2.5 g/L (preferably 2.0 g/L); the modification effect is better by controlling the dipping treatment temperature, time and dopamine concentration.
The specific preparation method of the epoxy resin curing agent solution comprises the following steps: mixing the epoxy resin, the curing agent, the coupling agent, the antioxidant and the ultraviolet absorbent at the temperature of not lower than 30 ℃, and standing in vacuum to obtain the epoxy resin-modified epoxy resin composition. Due to the fact that the epoxy resin (PE) is high in viscosity, the epoxy resin can keep fluidity by properly increasing the temperature, and air bubbles in the epoxy resin can be discharged.
The curing agent is preferably a toughening curing agent SH-200/201, and the curing agent has the characteristic of toughening epoxy resin, so that the defect that an epoxy resin matrix is easy to break due to the characteristic of hardness and brittleness in processing is relieved; meanwhile, the curing agent selected by the invention also has the characteristic of secondary curing, and provides possibility for subsequent secondary curing molding.
The specific processing conditions of vacuum standing are as follows: standing for 3-6 min (preferably 5min) under the relative vacuum degree of-20 Pa to promote the discharge of air bubbles in the resin.
The specific method for the dipping and laminating pressurization treatment comprises the following steps: laying aramid fiber fabrics on a substrate, coating an epoxy resin curing agent solution, preferably coating along the fiber direction of the aramid fiber fabrics to obtain a composite prepreg, and discharging redundant resin when each layer is stacked until all aramid fiber fabrics are stacked; and sealing and vacuumizing the stacked composite prepreg and the substrate, draining excess resin liquid between layers and enabling air bubbles in the resin to escape.
The substrate is preferably a transparent glass substrate, so that the coating state of the fiber cloth can be effectively observed, and uneven resin infiltration is avoided.
The pre-curing treatment conditions are specifically as follows: curing at 110-130 deg.C for 0.8-1.5 h (preferably 1 h).
And before the pre-curing treatment, the vacuumized composite prepreg is compacted, and the thickness of a stacking layer is controlled to be an mm, wherein a is the thickness of a single-layer aramid fiber fabric, n is the number of stacking layers, and n is 15-30 (preferably 20).
The compaction treatment is specifically compaction by using a compaction device (such as a steel plate); and further clamped using a clamp (e.g., an F-clamp).
The specific method for thickening the surface layer comprises the following steps: and (3) arranging pad thick layers on the upper surface and the lower surface of the preformed material, naturally clamping by using a substrate, and injecting the epoxy resin curing agent solution into the substrate by adopting a vacuum infusion method to increase the thickness of the surface layer of the preformed material.
The gasket is preferably used as the thick gasket layer, the gaskets are respectively arranged at four corners of the upper surface and the lower surface of the preformed material, and gaps are naturally formed between the substrate and the upper surface and the lower surface of the preformed material due to the blocking effect of the gaskets, so that the epoxy resin curing agent solution can be covered on the surface of the preformed material during subsequent vacuum infusion, and the surface layer is thickened, therefore, the substrate is further preferably used for fixing the preformed material in a vertical mode; meanwhile, because the hardness of the preformed material matrix is not high, the gasket can sink into the matrix under the action of vacuum negative pressure, and the thickness of the gasket is larger than that of the surface matrix.
The secondary curing temperature is 140-160 ℃ (preferably 150 ℃), and the curing treatment time is 3.5-5 h (preferably 4 h).
The aramid fiber reinforced epoxy resin matrix composite material prepared by the method has the aramid fiber content of 65-70% by mass and the resin content of 30-35% by mass.
The invention has the beneficial effects that:
(1) the aramid fiber reinforced epoxy resin matrix composite material prepared by the invention has high fiber content (the aramid fiber content can be up to more than 65%) and high surface layer matrix thickness, improves the mechanical property of the composite material, effectively reduces or even avoids the phenomena of layering, burr and tearing of the composite material in the subsequent processing process, and improves the processability of the composite material.
(2) The preparation process is simple, and the processability of the material difficult to process is improved from the aspect of material characteristics; does not need to update equipment, is convenient for popularization in the industry and has good practical application value.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a diagram of a machined edge burr generation and suppression mechanism; wherein, 1 is a processing cutter, 2 is a composite material fiber layer, and 3 is a resin matrix layer.
FIG. 2 is a schematic view of the pre-cure process clamping; wherein, 4 is a metal pressing plate, 5 is an F clamp, 6 is a vacuum bag, 7 is a fiber laying layer stacking object, and 8 is a glass substrate.
FIG. 3 is a schematic view of a secondary curing process clamp; wherein, 4 is the metal clamp plate, 7 is fibre and spreads the layer stack thing, 9 is the thickening of top layer base member and reserves the space, 8 is the glass substrate.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise. It is to be understood that the scope of the invention is not to be limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
As mentioned above, due to the high strength and toughness of the fibers, the material exhibits mechanical anisotropy, and defects including delamination, burrs and tears are common in processing. Meanwhile, the existing aramid fiber composite material plate is generally low in fiber content, the mass percentage of the existing aramid fiber composite material plate is only 30% -40%, the surface layer thickness of the plate is close to the interlayer thickness, an extremely thin matrix cannot provide enough support for fibers in the processing process, the fibers are easy to break, the fibers are more difficult to cut, and the processing quality is further deteriorated.
In view of the above, in one embodiment of the present invention, an aramid fiber reinforced epoxy resin matrix composite is provided, which includes the following raw materials in parts by mass:
65-70 parts of modified aramid fiber, 30-35 parts of epoxy resin, 8-12 parts of curing agent, 1-2 parts of coupling agent and 0.5-1 part of antioxidant and ultraviolet absorbent.
The modified aramid fiber is dopamine modified aramid fiber, preferably, the modification treatment time is 2 hours, and the dopamine concentration is 2 g/L;
the curing agent is an epoxy resin curing agent, and is further preferably SH-200/201;
the coupling agent is: a silane coupling agent kh560 added only to the epoxy resin;
the antioxidant is as follows: V73-P; the ultraviolet absorbent is: UV-196, the two are used in combination, and the ratio of the two is not particularly limited.
In another embodiment of the invention, the thickness of the surface matrix of the aramid fiber reinforced epoxy resin matrix composite material is not less than 250 μm; the thickness of the matrix between the aramid fiber fabric layers is not more than 10 mu m.
In another embodiment of the present invention, there is provided a method for preparing an aramid fiber reinforced epoxy resin matrix composite material, the method comprising:
s1, aramid fiber modification: the dopamine is used for carrying out surface modification on the aramid fiber fabric, so that the interfacial property of the aramid fiber/epoxy resin is improved.
S2, preparing an epoxy resin curing agent solution: uniformly mixing epoxy resin, a curing agent, a coupling agent, an antioxidant and an ultraviolet absorbent, and then carrying out vacuum drying for later use;
s3, coating and stacking: arranging a substrate for coating and stacking aramid fiber fabrics, wherein the aramid fiber fabrics are coated along the fiber direction during coating; bagging the stacked materials together with the substrate, sealing, vacuumizing, discharging interlayer resin liquid and enabling bubbles in the resin to escape; pressing the vacuum bag up and down by using a steel plate, and clamping by using an F clamp;
s4, precuring: heating and pre-curing the stacked material;
s5, thickening the surface layer: after the pre-cured material is taken out, gaskets are respectively arranged at four corners of the front surface and the back surface, the pre-cured material is fixed by a substrate in a vertical mode, and the pre-cured material and the substrate are sealed by a vacuum bag; the thickness of the surface layer of the material is strengthened by using a vacuum infusion method;
s6, secondary curing: and (4) carrying out secondary heating and curing on the vacuum bag, taking out the vacuum bag after cooling at normal temperature, and dismantling the auxiliary clamp device.
It should be noted that, the steps S1 and S2 do not have a precedence order;
in another embodiment of the present invention, in step S1, a polydopamine coating is deposited on the surface of the aramid fiber by using oxidative autopolymerization of dopamine, so as to improve the interfacial properties of the aramid fiber/epoxy resin. The modification treatment temperature is 45-55 ℃ (preferably 50 ℃), the modification treatment time is 1.5-3 h (preferably 2h), and the fiber is taken out and subjected to ultrasonic cleaning to remove the unbound dopamine on the surface of the fiber; the concentration of the dopamine is 1.8-2.5 g/L (preferably 2.0g/L, anhydrous ethanol solution).
In another embodiment of the present invention, in step S2, the process flow should not be lower than 30 ℃ due to the high viscosity of the epoxy resin (PE), and the proper increase of the temperature is beneficial to maintain the fluidity of the epoxy resin and to discharge the bubbles in the resin.
In still another embodiment of the present invention, the curing agent is a toughening curing agent SH-200/201. The prepared solution is poured into the tray in time, so that the curing reaction can be prevented from being performed too fast.
In another embodiment of the present invention, in step S3, the coating state of the fiber cloth can be effectively observed by using the transparent glass substrate, thereby avoiding uneven resin impregnation.
In another embodiment of the present invention, in the step S4, the thickness of the aramid fiber cloth is about 0.2mm, the stacking thickness of the material is controlled to be 0.2 nmm (n is the number of stacking layers) by the related clamping device, the pre-curing temperature is 110 to 130 ℃ (preferably 120 ℃), and the curing treatment time is 0.8 to 1.5h (preferably 1 h).
In another embodiment of the present invention, in step S5, since the hardness of the pre-cured substrate is not high, in order to ensure that the thickness of the surface substrate reaches 250 μm, practical experience verifies that a 500 μm spacer is used, and the spacer will partially sink into the substrate under the vacuum negative pressure.
In another embodiment of the present invention, in the step S6, the curing temperature is 140 to 160 ℃ (preferably 150 ℃), and the curing time is 3.5 to 5 hours (preferably 4 hours).
In addition, the special toughening curing agent SH-200/201 capable of being cured for the second time is obtained by optimization screening. Due to the characteristics of the curing agent, the possibility is provided for a secondary curing molding process. Meanwhile, the curing agent has the characteristic of toughening the epoxy resin, so that the defect that an epoxy resin matrix is easy to break due to the characteristic of hardness and brittleness in processing is overcome.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
An aramid fiber reinforced epoxy resin matrix composite material is specifically prepared by the following steps:
1. modifying aramid fiber cloth fabric: adding dopamine into absolute ethyl alcohol, adjusting the concentration to 2g/L, soaking aramid fiber fabric in an absolute ethyl alcohol solution, heating in a water bath at 50 ℃ for 2h, taking out, and then ultrasonically cleaning to remove the unbound dopamine on the fiber surface.
2. Preparing an epoxy resin solution: the mass ratio is 32: 9: 1: 0.5: 0.5 epoxy resin (PE), a toughening curing agent SH-200/201, a silane coupling agent kh560, an antioxidant V73-P and an ultraviolet absorber UV-196 are mixed. After fully stirring, vacuumizing (relative vacuum degree-20 pa) in a vacuum drying kettle and standing for 5min to enable bubbles contained in the resin to escape.
3. Stacking fiber fabrics: impregnating aramid fiber fabrics with an epoxy resin solution, stacking, bagging and vacuumizing. And clamping by using a steel plate and an F clamp, and controlling the thickness of the stacked material to be 0.2n mm, wherein the thickness of the aramid fiber cloth is 0.2mm, n is the number of layers of the fiber fabric, and n is 20.
4. Pre-curing: curing at the primary curing temperature of 120 ℃ for 1 h.
5. Thickening the surface layer: the pre-cured material of the double-sided pad with the 0.5mm gasket is used, the glass substrate is used for naturally clamping the back sleeve bag, the vertical fixation is adopted, and the vacuum infusion method is used for increasing the thickness of the surface layer of the material.
6. Secondary curing: curing for 4h at 150 ℃ of secondary curing.
And taking out the aramid fiber composite material, and removing the resin material at the edge to obtain the prepared aramid fiber composite material. The aramid fiber reinforced epoxy resin matrix composite material comprises 65 mass percent of aramid fiber, 30 mass percent of resin, 250 mu m of surface layer matrix and 8 mu m of fiber interlayer matrix.
Example 2
An aramid fiber reinforced epoxy resin matrix composite material is specifically prepared by the following steps:
1. modifying aramid fiber cloth fabric: adding dopamine into absolute ethyl alcohol, adjusting the concentration to 2g/L, soaking aramid fiber fabric in an absolute ethyl alcohol solution, heating in a water bath at 50 ℃ for 2h, taking out, and then ultrasonically cleaning to remove the unbound dopamine on the fiber surface.
2. Preparing an epoxy resin solution: the mass ratio is 30: 10: 1.5: 0.3: 0.4 epoxy resin (PE), a toughening curing agent SH-200/201, a silane coupling agent kh560, an antioxidant V73-P and an ultraviolet absorber UV-196 are mixed. After fully stirring, vacuumizing (relative vacuum degree-20 pa) in a vacuum drying kettle and standing for 5min to enable bubbles contained in the resin to escape.
3. Stacking fiber fabrics: impregnating aramid fiber fabrics with an epoxy resin solution, stacking, bagging and vacuumizing. And clamping by using a steel plate and an F clamp, and controlling the thickness of the stacked material to be 0.2n mm, wherein the thickness of the aramid fiber cloth is 0.2mm, n is the number of layers of the fiber fabric, and n is 18.
4. Pre-curing: curing at the primary curing temperature of 120 ℃ for 1 h.
5. Thickening the surface layer: the pre-cured material of the double-sided pad with the 0.6mm gasket is used, the glass substrate is used for naturally clamping the back sleeve bag, the vertical fixation is adopted, and the vacuum infusion method is used for increasing the thickness of the surface layer of the material.
6. Secondary curing: curing for 4h at 150 ℃ of secondary curing.
And taking out the aramid fiber composite material, and removing the resin material at the edge to obtain the prepared aramid fiber composite material. The aramid fiber reinforced epoxy resin matrix composite material comprises 62 mass percent of aramid fiber, 34 mass percent of resin, 255 mu m of surface layer matrix and 9 mu m of fiber interlayer matrix.
Example 3
An aramid fiber reinforced epoxy resin matrix composite material is specifically prepared by the following steps:
1. modifying aramid fiber cloth fabric: adding dopamine into absolute ethyl alcohol, adjusting the concentration to 2g/L, soaking aramid fiber fabric in an absolute ethyl alcohol solution, heating in a water bath at 50 ℃ for 2h, taking out, and then ultrasonically cleaning to remove the unbound dopamine on the fiber surface.
2. Preparing an epoxy resin solution: according to the mass ratio of 35: 11: 2: 0.4: 0.3 epoxy resin (PE), a toughening curing agent SH-200/201, a silane coupling agent kh560, an antioxidant V73-P and an ultraviolet absorber UV-196 are mixed. After fully stirring, vacuumizing (relative vacuum degree-20 pa) in a vacuum drying kettle and standing for 5min to enable bubbles contained in the resin to escape.
3. Stacking fiber fabrics: impregnating aramid fiber fabrics with an epoxy resin solution, stacking, bagging and vacuumizing. And clamping by using a steel plate and an F clamp, and controlling the thickness of the stacked material to be 0.2n mm, wherein the thickness of the aramid fiber cloth is 0.2mm, n is the number of layers of the fiber fabric, and n is 22.
4. Pre-curing: curing at the primary curing temperature of 120 ℃ for 1 h.
5. Thickening the surface layer: the pre-cured material of the double-sided pad with the 0.5mm gasket is used, the glass substrate is used for naturally clamping the back sleeve bag, the vertical fixation is adopted, and the vacuum infusion method is used for increasing the thickness of the surface layer of the material.
6. Secondary curing: curing for 4h at 150 ℃ of secondary curing.
And taking out the aramid fiber composite material, and removing the resin material at the edge to obtain the prepared aramid fiber composite material. The aramid fiber reinforced epoxy resin matrix composite material contains 65 mass percent of aramid fiber, 32 mass percent of resin, 260 mu m of surface layer matrix and 9 mu m of fiber interlayer matrix.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (17)

1. The aramid fiber reinforced epoxy resin matrix composite material is characterized by comprising the following raw materials in parts by mass:
65-70 parts of modified aramid fiber, 30-35 parts of epoxy resin, 8-12 parts of curing agent, 1-2 parts of coupling agent and 0.5-1 part of antioxidant and ultraviolet absorbent;
the curing agent SH-200/201;
the preparation method of the aramid fiber reinforced epoxy resin matrix composite material comprises the following steps:
impregnating aramid fiber fabric subjected to dopamine modification treatment with an epoxy resin curing agent solution to obtain a composite prepreg, and heating and pre-curing the composite prepreg after laminating and pressurizing the composite prepreg to obtain a pre-cured material; under the condition that the epoxy resin in the pre-curing material is in a semi-solid state, pouring an epoxy resin curing agent into the pre-curing material by using a vacuum pouring method to thicken the surface layer of the pre-forming material, and then carrying out secondary curing to obtain the epoxy resin curing agent;
the specific method for the dipping laminating pressurization treatment comprises the following steps: laying aramid fiber fabrics on a substrate, coating an epoxy resin curing agent solution, coating along the fiber direction of the aramid fiber fabrics during coating to obtain a composite prepreg, and discharging redundant resin when each layer is stacked until all aramid fiber fabrics are stacked; sealing and vacuumizing the stacked composite prepreg and the substrate;
the specific method for thickening the surface layer comprises the following steps: setting pad thick layers on the upper and lower surfaces of the preformed material, naturally clamping by using a substrate, and injecting the epoxy resin curing agent solution into the substrate by adopting a vacuum infusion method to increase the thickness of the surface layer of the preformed material; the gasket thick layer is a gasket, and the gasket is respectively arranged at four corners of the upper surface and the lower surface of the preformed material.
2. The aramid fiber reinforced epoxy resin matrix composite material of claim 1, wherein the modified aramid fiber is a dopamine modified aramid fiber;
the coupling agent is: a silane coupling agent kh560 added only to the epoxy resin;
the antioxidant is V73-P; the ultraviolet absorbent is UV-196.
3. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 2, wherein the thickness of the matrix of the surface layer of the aramid fiber reinforced epoxy resin matrix composite material is not less than 250 μm; the thickness of the matrix between the aramid fiber fabric layers is not more than 10 mu m.
4. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 3, wherein the specific preparation method of the dopamine modified aramid fiber fabric comprises: soaking the aramid fiber fabric in a dopamine ethanol solution.
5. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 4,
the soaking temperature is controlled to be 45-55 ℃, the soaking time is controlled to be 1.5-3 h, and the concentration of dopamine is 1.8-2.5 g/L.
6. The aramid fiber reinforced epoxy resin matrix composite material according to claim 5, wherein the soaking treatment temperature is controlled to be 50 ℃, the soaking treatment time is controlled to be 2 hours, and the concentration of dopamine is 2.0 g/L.
7. The aramid fiber reinforced epoxy resin matrix composite material according to claim 1, wherein the specific preparation method of the epoxy resin curing agent solution comprises: mixing the epoxy resin, the curing agent, the coupling agent and the antioxidant at the temperature of not lower than 30 ℃, and standing in vacuum to obtain the epoxy resin.
8. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 7, wherein the specific processing conditions of vacuum standing are as follows: standing for 3-6 min under the vacuum degree of-20 Pa.
9. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 8, wherein the specific processing conditions of vacuum standing are as follows: standing at-20 Pa for 5 min.
10. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 1, wherein the substrate is a transparent glass substrate.
11. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 1, wherein the pre-curing treatment conditions are specifically: curing at 110-130 ℃ for 0.8-1.5 h.
12. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 11, wherein the pre-curing treatment conditions are specifically: curing for 1h at 110-130 ℃;
and before the pre-curing treatment, the vacuumized composite prepreg is compacted, and the thickness of a stacking layer is controlled to be an mm, wherein a is the thickness of a single-layer aramid fiber fabric, n is the number of stacking layers, and n is 15-30.
13. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 12, wherein the compacting process is in particular compacting with a compacting device and clamping with a clamp; n is 20.
14. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 1, wherein the preformed material is fixed in a vertical manner using a base plate; the thickness of the gasket is larger than that of the surface layer matrix.
15. The aramid fiber reinforced epoxy resin matrix composite material as claimed in claim 1, wherein the secondary curing temperature is 140-160 ℃ and the curing treatment time is 3.5-5 h.
16. The aramid fiber reinforced epoxy resin matrix composite material according to claim 15, wherein the secondary curing temperature is 150 ℃ and the curing treatment time is 4 h.
17. The aramid fiber reinforced epoxy resin matrix composite material as claimed in any one of claims 1 to 16, wherein the aramid fiber content in the aramid fiber reinforced epoxy resin matrix composite material is 65 to 70 mass% and the resin content is 30 to 35 mass%.
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CN110922616B (en) * 2019-12-12 2022-04-12 西安工业大学 Fiber reinforced polymer composite material and preparation method thereof
CN111118896A (en) * 2019-12-30 2020-05-08 浙江华正新材料股份有限公司 Modified aramid fiber and modified aramid fiber composite material
CN111793323A (en) * 2020-04-09 2020-10-20 上海大学 Thermosetting resin-based aramid fiber composite material and preparation method thereof
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CN113292822B (en) * 2021-05-24 2022-07-15 安徽工程大学 Aramid fiber-epoxy resin based composite material and preparation method and application thereof
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