CN114477797B - Basalt fiber surface modification method - Google Patents

Basalt fiber surface modification method Download PDF

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CN114477797B
CN114477797B CN202210091378.1A CN202210091378A CN114477797B CN 114477797 B CN114477797 B CN 114477797B CN 202210091378 A CN202210091378 A CN 202210091378A CN 114477797 B CN114477797 B CN 114477797B
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basalt fiber
deionized water
drying
basalt
cleaning
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CN114477797A (en
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武清
邓昊
白换换
叶紫怡
朱建锋
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Shaanxi University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/465Coatings containing composite materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/26Macromolecular compounds or prepolymers
    • C03C25/32Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/26Macromolecular compounds or prepolymers
    • C03C25/32Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C03C25/328Polyamides
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/40Organo-silicon compounds
    • 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
    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/06Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/10Silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/08Ingredients agglomerated by treatment with a binding agent
    • 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a basalt fiber surface modification method, which comprises the following steps: 1) Surface degerming treatment of basalt fibers; 2) Uniformly dispersing the degerming basalt fiber treated in the step 1) in a mixed solution of an aminosilane coupling agent, ethanol and deionized water, reacting for 2-4 hours at 50-70 ℃, then cleaning with deionized water, and drying for later use; 3) Dipping basalt fibers treated in the step 2) into a phytic acid aqueous solution, then cleaning with deionized water, and drying for later use; 4) Dipping the basalt fiber treated in the step 3) into an amino-terminated polymer organic solution, then cleaning with deionized water, and drying to obtain the modified basalt fiber. The method provided by the invention is simple, environment-friendly, efficient and easy to popularize in a large scale, and the interface bonding strength of the reinforced epoxy composite material can be improved by 19.6% -90.8% by utilizing the modified basalt fiber prepared by the invention.

Description

Basalt fiber surface modification method
Technical Field
The invention relates to a surface and interface modification technology of a material, in particular to a basalt fiber surface modification method.
Background
The basalt fiber is a high-performance inorganic silicate fiber which is prepared by directly melting and wiredrawing basalt ore, and the main components of the basalt fiber are silicon dioxide, aluminum oxide, calcium oxide and the like, and because other alkali metal oxides are not discharged in the melting process of the basalt ore, and new components are not required to be added, the manufacturing process of the basalt fiber does not influence and pollute the human body and the nature, and the basalt fiber is called as novel environment-friendly fiber in the 21 st century. The basalt fiber has the advantages of good mechanical property, high temperature resistance, acid and alkali resistance, low hygroscopicity, good insulativity, heat insulation and sound insulation performance, good wave permeability and the like, but some defects of the basalt fiber also affect the wide application of the basalt fiber in the field of composite materials, one of the problems which have been plagued is that the surface of the basalt fiber is smooth, the surface of the basalt fiber presents chemical inertness, the interface combination between the basalt fiber and resin is poor when the basalt fiber is used as a reinforcing body of a resin-based composite material, the transmission of stress from the resin to the fiber is not facilitated, and the prepared composite material is difficult to fully exert the excellent mechanical property of the basalt fiber. Therefore, the surface modification of basalt fibers is particularly important.
At present, the common basalt fiber surface modification methods comprise a plasma treatment method, an acid-base treatment method and a nanoparticle modification method, however, the methods generally have the problems of complex preparation process, easiness in environmental pollution and inconvenience in large-scale application.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a basalt fiber surface modification method which is simple, environment-friendly, efficient, low in cost and easy for mass production, and the modified basalt fiber prepared by the method can effectively improve the interface bonding strength of the basalt fiber reinforced epoxy composite material.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a basalt fiber surface modification method comprises the following steps:
1) Surface degerming treatment of basalt fibers; heating basalt fiber in acetone solution, condensing and refluxing, then cleaning with deionized water, and vacuum drying for standby;
2) Uniformly dispersing the degerming basalt fiber treated in the step 1) in a mixed solution of an aminosilane coupling agent, ethanol and deionized water, reacting for 2-4 hours at 50-70 ℃, then cleaning with deionized water, and drying for later use;
3) Dipping basalt fibers treated in the step 2) into a phytic acid aqueous solution, then cleaning with deionized water, and drying for later use;
4) Dipping the basalt fiber treated in the step 3) into an amino-terminated polymer organic solution, then cleaning with deionized water, and drying to obtain the modified basalt fiber.
Further, the temperature of the condensation reflux in the step 1) is 80-100 ℃, and the time of the condensation reflux is 12-48 hours.
Further, the aminosilane coupling agent in the step 2) is 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, 3-aminopropyl methyldiethoxysilane or 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane.
Further, the mass ratio of the aminosilane coupling agent, the absolute ethyl alcohol and the deionized water in the mixed solution of the aminosilane coupling agent, the ethyl alcohol and the deionized water in the step 2) is 1:4 (0.1-0.5).
Further, the mass ratio of the phytic acid to the deionized water in the phytic acid aqueous solution in the step 3) is (0.05-0.5) to 100.
Further, the amino-terminated polymer in the step 4) is liquid polyetherimide, liquid polyamide-amine type dendrimer, liquid polydopamine, liquid polyetheramine or liquid polypropylene imine.
Further, the organic solvent of the amino-terminated polymer organic solution in the step 4) is acetone, absolute ethyl alcohol, tetrahydrofuran, dimethylformamide or dichloromethane.
Further, the volume ratio of the amino-terminated polymer to the organic solvent in the amino-terminated polymer organic solution in the step 4) is (0.5-5): 100.
Further, the temperature of the vacuum drying in the step 1) and the drying in the steps 2), 3) and 4) is 40-80 ℃, and the drying time is 2-5 hours.
Further, the time of soaking in the steps 3) and 4) is 5-30 min.
Compared with the prior art, the invention has the following technical effects:
(1) The invention combines the environment-friendly basalt fiber with the bio-based modified material for the first time, so that the basalt fiber surface modification method is simple, environment-friendly, low in cost, high in efficiency and capable of being popularized and applied in large scale.
(2) The modified basalt fiber reinforced epoxy resin prepared by the method can improve the interfacial bonding strength of the composite material by 19.6-90.8%.
(3) The reinforcing mechanism for improving the bonding strength of the composite material interface is as follows: the amino silane coupling agent, the phytic acid and the amino-terminated polymer can form a stable high-density cross-linked ionic bonding network in the interface area of the composite material, and covalent bonds and hydrogen bonds can be formed between the amino-terminated polymer and the epoxy resin, so that the mode of multiple interactions of the ionic bonds, the covalent bonds and the hydrogen bonds is favorable for interface stress transmission so as to improve the interface bonding strength of the composite material. In addition, the composition of the aminosilane coupling agent, the phytic acid and the amino-terminated polymer can improve the surface roughness of basalt fibers, improve the wettability of the basalt fibers and epoxy resin, and facilitate the full contact of the fibers and the resin so as to promote the adhesion of the basalt fibers and the resin.
Drawings
FIG. 1 is a surface topography of basalt fiber treated in step 1) in example 1 of the present invention;
FIG. 2 is a surface topography of the modified basalt fiber prepared in example 1 of the present invention;
FIG. 3 is a surface topography of a modified basalt fiber prepared in example 2 of the present invention;
FIG. 4 is a surface topography of a modified basalt fiber prepared in example 3 of the present invention.
Detailed Description
The following examples illustrate the invention in further detail.
Example 1
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 100 ℃ to condense and reflux 12 h, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 40 ℃ for 5 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3-aminopropyl trimethoxy silane, absolute ethyl alcohol and deionized water in a mass ratio of 1:4:0.1, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 50 ℃ for 4h, cleaning the degerming basalt fiber with deionized water, drying in a drying oven at 40 ℃ for 5 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.05:100 for 5min, then cleaning with deionized water, drying in a drying oven at 40 ℃ for 5h, and taking out for later use;
4) Dipping the basalt fiber obtained by the treatment in the step 3) in a liquid organic solution of the polypropylene imine and the dimethyl formamide with the volume ratio of 0.5:100 for 5min, then cleaning with deionized water, and drying in a drying oven at 40 ℃ for 5h to obtain the modified basalt fiber.
FIG. 1 is a surface topography of degerming basalt fiber obtained by degerming treatment in step 1) in the embodiment; FIG. 2 is a surface topography of the modified basalt fiber prepared in this example; as can be seen from fig. 1 and 2, the degerming basalt fiber (shown in fig. 1) has a smooth surface, in contrast, the surface of the modified basalt fiber is uniformly coated with a coating, and a few high polymer bulges are visible. The study shows that the interface bonding strength of the modified basalt fiber reinforced epoxy composite material prepared by the embodiment is improved by 30.4 percent compared with that of the degerming basalt fiber reinforced epoxy composite material.
Example 2
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 80 ℃ to condense and reflux 48 and h, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 60 ℃ for 3 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3-aminopropyl triethoxysilane, anhydrous ethanol and deionized water in a mass ratio of 1:4:0.3, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 60 ℃ for 3h, cleaning the degerming basalt fiber with deionized water, drying in a drying oven at 60 ℃ for 3 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.1:100 for 30min, then cleaning with deionized water, drying in a drying oven at 60 ℃ for 3h, and taking out for later use;
4) Dipping the basalt fiber obtained by the treatment in the step 3) in a liquid polyetherimide and absolute ethyl alcohol organic solution with the volume ratio of 1:100 for 30min, then cleaning with deionized water, and drying in a drying oven at 60 ℃ for 3h to obtain the modified basalt fiber.
FIG. 3 is a surface topography of the modified basalt fiber prepared in this example; the figure shows that the surface of the basalt fiber after modification is uniformly coated by the coating, and more high polymer bulges are visible. Research shows that the interface bonding strength of the modified basalt fiber reinforced epoxy composite material prepared by the embodiment is improved by 75.0% compared with that of the degerming basalt fiber reinforced epoxy composite material.
Example 3
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 90 ℃ to condense and reflux 24 h, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 80 ℃ for 2 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3-aminopropyl methyl diethoxy silane, absolute ethyl alcohol and deionized water in a mass ratio of 1:4:0.5, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 70 ℃ for 2h, cleaning the degerming basalt fiber with deionized water, drying in a drying oven at 80 ℃ for 2 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.2:100 for 15min, then cleaning with deionized water, drying in a drying oven at 80 ℃ for 2h, and taking out for later use;
4) Dipping basalt fiber obtained in the step 3) in a liquid polyetheramine and polyetheramine organic solution with the acetone volume ratio of 3:100 for 15min, then cleaning with deionized water, and drying in a drying oven at 80 ℃ for 2h to obtain modified basalt fiber.
Fig. 4 is a surface morphology diagram of the modified basalt fiber prepared in this example, and it can be seen from the figure that the surface of the modified basalt fiber is uniformly coated with a coating, and the surface of the fiber is covered with polymer protrusions. Research shows that the interface bonding strength of the modified basalt fiber reinforced epoxy composite material prepared by the embodiment is improved by 19.6% compared with that of the degerming basalt fiber reinforced epoxy composite material.
Example 4
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 80 ℃ to condense and reflux 24 h, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 70 ℃ for 4 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3-aminopropyl triethoxysilane, absolute ethyl alcohol and deionized water in a mass ratio of 1:4:0.2, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 60 ℃ for 4h, cleaning the degerming basalt fiber with deionized water, drying the degerming basalt fiber in a drying oven at 70 ℃ for 4 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.3:100 for 25min, then cleaning with deionized water, drying in a drying oven at 70 ℃ for 4h, and taking out for later use;
4) Dipping the basalt fiber obtained in the step 3) in a liquid polydopamine and tetrahydrofuran organic solution with the volume ratio of 2:100 for 25min, then cleaning with deionized water, and drying in a drying oven at 70 ℃ for 4h to obtain the modified basalt fiber.
Research shows that the interface bonding strength of the modified basalt fiber reinforced epoxy composite material prepared by the embodiment is improved by 90.8% compared with that of the degerming basalt fiber reinforced epoxy composite material.
Example 5
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 90 ℃ for condensation reflux for 48 hours, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 50 ℃ for 5 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3- [2- (2-amino ethylamino) ethylamino ] propyl-trimethoxy silane, absolute ethyl alcohol and deionized water in a mass ratio of 1:4:0.5, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 50 ℃ for 2h, cleaning the degerming basalt fiber with deionized water, drying at 50 ℃ in a drying box for 5 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.5:100 for 10min, then cleaning with deionized water, drying in a drying oven at 50 ℃ for 5h, and taking out for later use;
4) Dipping basalt fiber obtained in the step 3) in a liquid polyamide-amine dendritic polymer and methylene dichloride solution with the volume ratio of 5:100 for 10min, then cleaning with deionized water, and drying in a drying box at 50 ℃ for 5h to obtain modified basalt fiber.
The study shows that the interface bonding strength of the modified basalt fiber reinforced epoxy composite material prepared by the embodiment is improved by 54.3 percent compared with that of the degerming basalt fiber reinforced epoxy composite material.
Example 6
The embodiment provides a basalt fiber surface modification method, which comprises the following steps:
1) Placing basalt fiber tows in an acetone solution with the temperature of 90 ℃ for condensation reflux for 36 hours, then cleaning the tows with deionized water, drying the tows in a vacuum drying oven at the temperature of 50 ℃ for 5 hours, and taking out the tows for later use;
2) Placing the degerming basalt fiber obtained in the step 1) into a mixed solution of 3- [2- (2-amino ethylamino) ethylamino ] propyl-trimethoxy silane, absolute ethyl alcohol and deionized water in a mass ratio of 1:4:0.4, carrying out ultrasonic treatment to uniformly disperse the degerming basalt fiber, reacting at 70 ℃ for 4h, cleaning the degerming basalt fiber with deionized water, drying the degerming basalt fiber in a drying oven at 80 ℃ for 2 hours, and taking out the degerming basalt fiber for later use;
3) Dipping basalt fibers obtained in the step 2) in a phytic acid aqueous solution with the mass ratio of phytic acid to deionized water of 0.4:100 for 10min, then cleaning with deionized water, drying in a drying oven at 50 ℃ for 3h, and taking out for later use;
4) Dipping basalt fiber obtained in the step 3) in a liquid polyamide-amine dendritic polymer and a polyamide-amine dendritic polymer organic solution with the volume ratio of dichloromethane solution of 4:100 for 20min, then cleaning with deionized water, and drying in a drying oven at 60 ℃ for 5h to obtain modified basalt fiber.

Claims (9)

1. The basalt fiber surface modification method is characterized by comprising the following steps of:
1) Surface degerming treatment of basalt fibers; heating basalt fiber in acetone solution, condensing and refluxing, then cleaning with deionized water, and vacuum drying for standby;
2) Uniformly dispersing the degerming basalt fiber treated in the step 1) in a mixed solution of an aminosilane coupling agent, ethanol and deionized water, reacting for 2-4 hours at 50-70 ℃, then cleaning with deionized water, and drying for later use;
3) Dipping basalt fibers treated in the step 2) into a phytic acid aqueous solution, then cleaning with deionized water, and drying for later use;
4) Dipping the basalt fiber treated in the step 3) into an amino-terminated polymer organic solution, then cleaning with deionized water, and drying to obtain modified basalt fiber;
the amino-terminated polymer is polyetherimide, polyamide-amine type dendritic polymer, polydopamine, polyetheramine or polypropyleneimine.
2. The basalt fiber surface modification method according to claim 1, wherein the condensation reflux temperature in the step 1) is 80-100 ℃, and the condensation reflux time is 12-48 hours.
3. The method for modifying the surface of basalt fiber according to claim 1, wherein the aminosilane coupling agent in the step 2) is 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, 3-aminopropyl methyldiethoxysilane or 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane.
4. The basalt fiber surface modification method of claim 1, wherein the mass ratio of the aminosilane coupling agent, the absolute ethyl alcohol and the deionized water in the mixed solution of the aminosilane coupling agent, the ethyl alcohol and the deionized water in the step 2) is 1:4 (0.1-0.5).
5. The method for modifying the surface of basalt fiber according to claim 1, wherein the mass ratio of the phytic acid to deionized water in the phytic acid aqueous solution in the step 3) is (0.05-0.5): 100.
6. The method for modifying the surface of basalt fiber according to claim 1, wherein the organic solvent of the organic solution of the amino-terminated polymer in the step 4) is acetone, absolute ethyl alcohol, tetrahydrofuran, dimethylformamide or methylene chloride.
7. The method of modifying basalt fiber surfaces according to claim 1, wherein the volume ratio of the amino-terminated polymer in the organic solution of the amino-terminated polymer in the step 4) to the organic solvent is (0.5-5): 100.
8. The method for modifying the surface of basalt fiber according to claim 1, wherein the temperature of the vacuum drying in the step 1) and the drying in the steps 2), 3) and 4) is 40 to 80 ℃, and the drying time is 2 to 5 hours.
9. The basalt fiber surface modification method according to claim 1, wherein the dipping time in the steps 3) and 4) is 5 to 30 minutes.
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CN115160608B (en) * 2022-08-22 2023-05-26 四川大学 Basalt fiber reinforced polyether-ether-ketone based composite material, and preparation method and application thereof
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