CN111363989A - Preparation method of fiber reinforced composite material - Google Patents

Preparation method of fiber reinforced composite material Download PDF

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Publication number
CN111363989A
CN111363989A CN201811588216.9A CN201811588216A CN111363989A CN 111363989 A CN111363989 A CN 111363989A CN 201811588216 A CN201811588216 A CN 201811588216A CN 111363989 A CN111363989 A CN 111363989A
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CN
China
Prior art keywords
fiber
composite material
reinforced composite
drying
coupling agent
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Pending
Application number
CN201811588216.9A
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Chinese (zh)
Inventor
王辉
王杰
王永霞
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Changchun A&z Science Co ltd
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Changchun A&z Science Co ltd
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Priority to CN201811588216.9A priority Critical patent/CN111363989A/en
Publication of CN111363989A publication Critical patent/CN111363989A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02Pretreatment of the fibres or filaments
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C47/00Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02Pretreatment of the fibres or filaments
    • C22C47/04Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C22C49/04Light metals
    • C22C49/06Aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C49/00Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

Abstract

The invention discloses a preparation method of a fiber reinforced composite material, belongs to the technical field of composite materials, and solves the technical problems of poor adhesive force, poor tensile resistance and the like when basalt fibers are adopted to prepare the fiber reinforced composite material. The preparation method of the fiber reinforced composite material provided by the invention adopts acetic acid pretreatment, titanate coupling agent and nano Al2O3Modifying the basalt fiber with titanate coupling agent to obtain fiber reinforced composite material, and cuttingThe specification of a broken sample is 300.0mm × 300.0.0 mm, the tensile strength is over 3500Mpa which is 7-9 times of that of steel, the tensile elastic modulus is 23000-43000 Mpa which is higher than that of steel, and the specific strength, namely the ratio of the strength of the material to the density thereof can reach 2000 Mpa/(g/cm) by adopting the prior art to detect3) The above.

Description

Preparation method of fiber reinforced composite material
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of a fiber reinforced composite material.
Background
Fiber Reinforced composite (FRP) is a composite formed by winding, molding or pultrusion a reinforcing Fiber material, such as glass Fiber, carbon Fiber, aramid Fiber, etc., with a matrix material. Common fiber-reinforced composites are classified into glass fiber reinforced composites (GFRP), carbon fiber reinforced Composites (CFRP), and aramid fiber reinforced composites (AFRP) according to the reinforcing material.
With the continuous progress of science and technology, environmental problems are more and more emphasized by people, and the sustainable and pollution-free green environmental material is gradually emphasized by people by inheriting the sustainable green exhibition concept. Unlike some materials used in the past, the green environmental materials do not destroy the existing ecological environment while maintaining good performance. The environment is not destructively affected in the whole process of using the environmental material. The discovery and use of environmental materials is therefore becoming the latest direction of research in materials disciplines.
Fiber reinforced polymer composites, particularly natural fibers, that are sustainable in environmental materials are of interest. Among them, Basalt is an excellent natural raw material, and it is ubiquitous in every corner of the earth, so that it is cheap, and is favorable for the wide production and application of Basalt fiber (Basalt fiber, abbreviated as BF). The basalt stone material has a very special structure which is composed of several oxides such as silicon dioxide and the like, so that the basalt fiber produced by the basalt stone material has excellent performance. The basalt fiber which is a green environment-friendly material has good mechanical property, high temperature resistance, excellent stability, chemical resistance, easy processing, no toxicity, environmental protection and low price. However, the basalt fiber has a very smooth surface and at the same time exhibits chemical inertness on the surface, so that the adhesion to the substrate is poor.
Disclosure of Invention
The invention provides a preparation method of a fiber reinforced composite material aiming at the technical problems.
In order to achieve the above purpose, the invention provides the following technical scheme:
a method of preparing a fiber-reinforced composite material, comprising the steps of:
(1) cleaning basalt fibers to remove impurities on the surfaces of the basalt fibers, and then drying the basalt fibers after suction filtration;
(2) adding 1mol/L acetic acid into the dried basalt fibers, stirring at 400-600 rpm for 60-90 min to disperse the basalt fibers, and then drying after suction filtration;
(3) adding ethyl acetate and a coupling agent into the acid-treated basalt fiber, stirring at 800-1200 rpm for 120-180 min, and then performing suction filtration and drying;
(4) taking nano Al2O3Dispersing the particles in deionized water, performing ultrasonic treatment at 30-50 Hz for 30-50 min, adjusting the pH value to 5.5-5.8 after the particles are fully dispersed, adding a silane coupling agent, stirring at room temperature at 1500-2000 rpm for 120-150 min for modification, performing centrifugal operation on the particles, washing with acetone for 2-3 times, and drying for later use;
(5) adding ethyl acetate and a coupling agent into the basalt fiber obtained in the step (3), standing for 5-10 minutes, and adding 20-30% of modified nano Al in percentage by volume2O3Stirring at 1500-2000 rpm for 120-150 min, pouring out the modified basalt fiber from the solution, filtering, cleaning and drying;
(6) pressing the modified basalt fiber at 700-800 MPa and 750-800 ℃ to prepare a prefabricated body;
(7) preheating and smelting the prefabricated body and the aluminum alloy in vacuum, maintaining the temperature at 800 ℃ for 120-150 min, and then filling inert gas for cooling and solidifying to obtain the fiber reinforced composite material.
Preferably, the cleaning method in the step (1) is as follows: and putting the basalt fiber into an acetone solution, and washing away surface impurities by adopting magnetic stirring for 30-50 min.
Preferably, the drying methods in steps (1) to (3) are all as follows: drying for 24-36 h at the temperature of 50-55 ℃.
Preferably, the drying methods in steps (4) and (5) are both: drying for 24-36 h at the temperature of 60-65 ℃.
Preferably, the coupling agent in the step (5) is a titanate coupling agent, and the volume fraction of the titanate coupling agent is 4-6% of that of the ethyl acetate.
Preferably, the inert gas in the step (7) is argon, and the pressure of the inert gas is 850-950 KPa.
Preferably, the silane coupling agent in the step (4) is 3-aminopropyltriethoxysilane, and the volume fraction of the silane coupling agent is 4-6% of deionized water.
Compared with the prior art, the invention has the beneficial effects that:
the basalt fiber serving as a novel green environment-friendly material has the advantages of good mechanical property, high temperature resistance, excellent stability, good chemical resistance, easiness in processing, no toxicity, environmental friendliness, low price and good low rolling resistance. Because the basalt fiber surface is characterized by hydrophilicity and lipophobicity, the binding force with a matrix is weak, the basalt fiber surface is easy to agglomerate, and in order to improve the mechanical property of the composite material while reducing loss factors, the preparation method of the fiber reinforced composite material provided by the invention firstly modifies the basalt fiber, can improve the filler dispersion in the matrix, prevents aggregation, and adopts ultrasonic waves to enhance the interface adhesiveness between the basalt fiber surface and the matrix. The titanate coupling agent can modify the surface of inorganic materials, and improve the dispersibility and filling amount of the filler. In addition, the physical and physicochemical properties of the fibrous filler and the fiber surface can be further improved by introducing foreign fillers such as nanoparticles, and the performance of the composite material is improved by adding the nanoparticles. The invention adopts acetic acid pretreatment, titanate coupling agent and nano Al2O3The basalt fiber is modified together with a titanate coupling agent, the cut sample specification of the finally obtained fiber reinforced composite material is 300.0mm × 300.0.0 mm, the tensile strength is over 3500Mpa detected by adopting the prior art, the tensile strength is 7-9 times of that of steel, the tensile elastic modulus is 23000-43000 Mpa and is also higher than that of steel, and the specific strength, namely the ratio of the strength of the material to the density thereof can reach 2000 Mpa/(g/cm)3) The above.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described in detail with reference to the following embodiments. The materials specifically mentioned are all commercially available products.
Example 1
The preparation method of the fiber reinforced composite material comprises the following steps:
(1) putting basalt fibers into an acetone solution, magnetically stirring for 30min to remove surface impurities, and then drying at 50 ℃ for 36h after suction filtration;
(2) adding 1mol/L acetic acid into the dried basalt fiber, stirring for 90min at 400 r/min to disperse the basalt fiber, and then drying for 24h at 55 ℃ after suction filtration;
(3) adding ethyl acetate and a coupling agent into the acid-treated basalt fiber, stirring for 180min at 800 r/min, and then drying for 36h at 50 ℃ after suction filtration;
(4) taking nano Al2O3Dispersing the particles in deionized water, performing ultrasonic treatment at 30Hz for 50min, adjusting the pH value to 5.5 after the particles are fully dispersed, adding 4% 3-aminopropyltriethoxysilane, stirring at room temperature for 150min at 1500 rpm for modification, centrifuging the particles, washing with acetone for 2 times, and drying at 60 deg.C for 36 h;
(5) adding ethyl acetate and 4% of titanate coupling agent into the basalt fiber obtained in the step (3), standing for 5 minutes, and adding 20% of modified nano Al in volume fraction2O3Stirring at 1500 rpm for 150min, pouring out the modified basalt fiber from the solution, filtering, cleaning, and drying at 60 deg.C for 36 h;
(6) taking the modified basalt fiber, and pressing the modified basalt fiber into a prefabricated body at the temperature of 750 ℃ under 700 MPa;
(7) preheating and smelting the prefabricated body and the aluminum alloy in vacuum, maintaining the temperature at 800 ℃ for 120min, and then filling 850KPa argon gas for cooling and solidifying to obtain the fiber reinforced composite material.
Example 2
The preparation method of the fiber reinforced composite material comprises the following steps:
(1) putting basalt fibers into an acetone solution, magnetically stirring for 40min to remove surface impurities, and then drying at 55 ℃ for 30h after suction filtration;
(2) adding 1mol/L acetic acid into the dried basalt fiber, stirring at 500 revolutions/min for 75min to disperse the basalt fiber, and then drying at 50 ℃ for 36h after suction filtration;
(3) adding ethyl acetate and a coupling agent into the acid-treated basalt fiber, stirring for 150min at 1000 r/min, and then drying for 24h at 55 ℃ after suction filtration;
(4) taking nano Al2O3Dispersing the particles in deionized water, performing ultrasonic treatment at 40Hz for 40min, adjusting the pH value to 5.7 after the particles are fully dispersed, adding 5% 3-aminopropyltriethoxysilane, stirring at 1800 rpm/min for 135min for modification, centrifuging the particles, washing with acetone for 3 times, and drying at 65 ℃ for 24h for later use;
(5) adding ethyl acetate and 5% of titanate coupling agent into the basalt fiber obtained in the step (3), standing for 8 minutes, and adding 25% of modified nano Al with volume fraction2O3Stirring at 1800 rpm for 135min, pouring out the modified basalt fiber from the solution, filtering, cleaning, and drying at 65 ℃ for 24 h;
(6) pressing the modified basalt fiber into a prefabricated body at 750MPa and 800 ℃;
(7) preheating and smelting the prefabricated body and the aluminum alloy in vacuum, maintaining the temperature at 800 ℃ for 135min, and then filling 800KPa argon gas for cooling and solidifying to obtain the fiber reinforced composite material.
Example 3
The preparation method of the fiber reinforced composite material comprises the following steps:
(1) putting basalt fibers into an acetone solution, magnetically stirring for 50min to remove surface impurities, and then drying at 55 ℃ for 24h after suction filtration;
(2) adding 1mol/L acetic acid into the dried basalt fiber, stirring at 600 revolutions/min for 60min to disperse the basalt fiber, and then drying at 55 ℃ for 24h after suction filtration;
(3) adding ethyl acetate and a coupling agent into the acid-treated basalt fiber, stirring at 1200 rpm for 120min, and then drying at 55 ℃ for 24h after suction filtration;
(4) taking nano Al2O3Dispersing the particles in deionized water, performing ultrasonic treatment at 50Hz for 30min, adjusting the pH value to 5.8 after the particles are fully dispersed, adding 6% 3-aminopropyltriethoxysilane, stirring at room temperature of 2000 rpm for 120min for modification, centrifuging the particles, washing with acetone for 2-3 times, and drying at 65 ℃ for 24h for later use;
(5) adding ethyl acetate and 6% of titanate coupling agent into the basalt fiber obtained in the step (3), standing for 10 minutes, and adding 30% of volume fraction of modified nano Al2O3Stirring at 2000 rpm for 120min, pouring out the modified basalt fiber from the solution, filtering, cleaning, and drying at 60-65 ℃ for 24-36 h;
(6) pressing the modified basalt fiber into a prefabricated body at 800MPa and 800 ℃;
(7) preheating and smelting the prefabricated body and the aluminum alloy in vacuum, maintaining the temperature at 800 ℃ for 150min, and then filling 950KPa argon gas for cooling and solidifying to obtain the fiber reinforced composite material.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: it is to be understood that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof, but such modifications or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (7)

1. A method for preparing a fiber reinforced composite material, comprising the steps of:
(1) cleaning basalt fibers to remove impurities on the surfaces of the basalt fibers, and then drying the basalt fibers after suction filtration;
(2) adding 1mol/L acetic acid into the dried basalt fibers, stirring at 400-600 rpm for 60-90 min to disperse the basalt fibers, and then drying after suction filtration;
(3) adding ethyl acetate and a coupling agent into the acid-treated basalt fiber, stirring at 800-1200 rpm for 120-180 min, and then performing suction filtration and drying;
(4) taking nano Al2O3Dispersing the particles in deionized water, performing ultrasonic treatment at 30-50 Hz for 30-50 min, adjusting the pH value to 5.5-5.8 after the particles are fully dispersed, adding a silane coupling agent, stirring at room temperature at 1500-2000 rpm for 120-150 min for modification, performing centrifugal operation on the particles, washing with acetone for 2-3 times, and drying for later use;
(5) adding ethyl acetate and a coupling agent into the basalt fiber obtained in the step (3), standing for 5-10 minutes, and adding 20-30% of modified nano Al in percentage by volume2O3Stirring at 1500-2000 rpm for 120-150 min, pouring out the modified basalt fiber from the solution, filtering, cleaning and drying;
(6) pressing the modified basalt fiber at 700-800 MPa and 750-800 ℃ to prepare a prefabricated body;
(7) preheating and smelting the prefabricated body and the aluminum alloy in vacuum, maintaining the temperature at 800 ℃ for 120-150 min, and then filling inert gas for cooling and solidifying to obtain the fiber reinforced composite material.
2. The method for preparing a fiber-reinforced composite material according to claim 1, wherein the cleaning method in the step (1) is: and putting the basalt fiber into an acetone solution, and washing away surface impurities by adopting magnetic stirring for 30-50 min.
3. The method for producing a fiber-reinforced composite material according to claim 1, wherein the drying method in each of the steps (1) to (3) is: drying for 24-36 h at the temperature of 50-55 ℃.
4. The method for preparing a fiber-reinforced composite material according to claim 1, wherein the drying method in steps (4) and (5) is: drying for 24-36 h at the temperature of 60-65 ℃.
5. The preparation method of the fiber reinforced composite material according to claim 1, wherein the coupling agent in the step (5) is a titanate coupling agent, and the volume fraction of the titanate coupling agent is 4-6% of ethyl acetate.
6. The method for preparing a fiber-reinforced composite material according to claim 1, wherein the inert gas in the step (7) is argon gas, and the pressure thereof is 850 to 950 KPa.
7. The method for preparing the fiber-reinforced composite material according to claim 1, wherein the silane coupling agent in the step (4) is 3-aminopropyltriethoxysilane, and the volume fraction of the silane coupling agent is 4-6% of deionized water.
CN201811588216.9A 2018-12-25 2018-12-25 Preparation method of fiber reinforced composite material Pending CN111363989A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN112110689A (en) * 2020-09-23 2020-12-22 四川鼎德商品混凝土有限公司 Ultrahigh-strength high-performance concrete and preparation method thereof
CN114573274A (en) * 2022-03-21 2022-06-03 江阴永盛交通工程有限公司 Anti-rutting regenerated asphalt mixture and processing technology thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112110689A (en) * 2020-09-23 2020-12-22 四川鼎德商品混凝土有限公司 Ultrahigh-strength high-performance concrete and preparation method thereof
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CN114573274A (en) * 2022-03-21 2022-06-03 江阴永盛交通工程有限公司 Anti-rutting regenerated asphalt mixture and processing technology thereof

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Application publication date: 20200703