CN110550870A - surface treatment method of basalt scale fibers - Google Patents
surface treatment method of basalt scale fibers Download PDFInfo
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- CN110550870A CN110550870A CN201910973384.8A CN201910973384A CN110550870A CN 110550870 A CN110550870 A CN 110550870A CN 201910973384 A CN201910973384 A CN 201910973384A CN 110550870 A CN110550870 A CN 110550870A
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- basalt
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/005—Surface treatment of fibres or filaments made from glass, minerals or slags by mechanical means
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/40—Organo-silicon compounds
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- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a surface treatment method of basalt scale fibers, relates to the field of surface treatment, and mainly solves the technical problems that the existing basalt scale fibers are poor in dispersibility in a polymer matrix and weak in binding force with the polymer matrix. The surface of the scale fiber is treated by adopting a silane coupling agent, a treatment process combining high-power ultrasound and high-speed shearing is adopted, so that a large number of organic functional groups are attached to the surface of the scale fiber, the scale fiber can be chemically bonded with a polymer matrix material, different active functional groups can be grafted on the surface of the scale fiber according to different polymer systems and application requirements, a special device is not used, high-temperature and high-pressure conditions are not needed, and the process is simple. The modified composite material has high interface compatibility, improved fiber aggregation and other advantages, and is suitable for use in preparing polymer base functional composite material.
Description
Technical Field
The invention relates to a surface treatment process of basalt scale fibers.
Background
The basalt fiber is mainly composed of SiO 2, Al 2 O 3, FeO, Fe 2 O 3, Na 2 O, K 2 O, CaO, MgO, TiO 2 and the like, wherein the SiO 2 and the Al 2 O 3 account for more than 70 percent.
The basalt flake is a novel basalt fiber, is in a transparent or dark green sheet-shaped structure, is generally about 3 mu m thick and is generally about 25-3 mm in size. Because the content of iron oxide, titanium dioxide, aluminum oxide and calcium oxide in the basalt flakes is high, the shielding effect can be generated, and the basalt flakes also have unique advantages in the aspects of acid-base resistance and corrosion resistance. When the existing composite material is prepared by utilizing basalt scales, the basalt scales are directly added into a polymer matrix to be mixed, and due to the scale structure of the basalt scales, the dispersion of the basalt scales in the polymer matrix is poor, the binding force with the polymer matrix is weak, and the comprehensive performance of the composite material is difficult to greatly improve.
Disclosure of Invention
the invention provides a surface treatment method of basalt scale fibers, aiming at solving the technical problems of poor dispersibility of the existing basalt scale in a polymer matrix and weak bonding force with the polymer matrix.
the invention relates to a surface treatment method of basalt scale fibers, which comprises the following steps:
firstly, adding a silane coupling agent into alcohol according to the mass percentage concentration of the silane coupling agent of 1-5% to obtain an alcohol solution of the silane coupling agent;
Secondly, adding basalt flake fibers into a coupling agent alcoholic solution to obtain a mixed solution; placing the mixed solution in a container, and carrying out high-speed shearing stirring for 20-60 min by using a high-speed shearing stirrer at the rotating speed of 1000-3000 rpm; then placing the mixture into an ultrasonic cleaning machine with the power of 300-700 w for ultrasonic dispersion for 20-60 min;
and thirdly, filtering the basalt scale fibers treated in the second step, washing with alcohol, drying the solvent, and standing at room temperature for 20-24 hours to complete the surface treatment of the basalt scale fibers.
the method comprises the steps of firstly, carrying out high-speed shearing dispersion and ultrasonic oscillation dispersion treatment on basalt scale fibers in an alcoholic solution of a silane coupling agent, increasing the contact between the scale fibers and the silane coupling agent, providing a sufficient reaction opportunity, carrying out etching on the surfaces of the basalt scale fibers through ultrasonic treatment, increasing the roughness and the surface area of the fibers, and promoting the silane coupling agent to be attached to the surfaces and the edges of the scales in a hydrogen bond mode. Then, the mixture is placed at room temperature for a sufficient period of time to contact with moisture in the air, and the silane coupling agent is hydrolyzed into silanol, which lays a good foundation for being capable of forming stable Si-O-bond connection with the inorganic component of the scale fibers. According to the invention, the surface and the edge of basalt scale fiber are modified by a large amount of organic functional groups, so that the interfacial compatibility of the basalt scale fiber is improved, the basalt scale fiber can be chemically bonded with a polymer matrix material, compared with the method that a coupling agent is directly added into resin, the pretreatment can effectively and uniformly modify the scale, the basalt scale fiber has a better infiltration effect in the resin, and the fiber agglomeration phenomenon is greatly improved due to the chemical bond formed with the resin interface, so that the performance of the polymer is improved, and the basalt scale fiber is suitable for preparing a polymer-based functional composite material.
The invention can graft different active functional groups on the surface of the scale fiber according to different polymer systems and application requirements, does not use a special device, does not need high temperature and high pressure conditions, has simple process and good operability. Is suitable for the field of preparation of polymer-based functional composite materials.
Drawings
FIG. 1 is an infrared spectrum of unmodified basalt flake fibers;
FIG. 2 is an infrared spectrum of a modified basalt flake fiber pattern of example 1;
FIG. 3 is an infrared spectrum of a modified basalt flake fiber pattern of comparative test 1;
FIG. 4 is an infrared spectrum of a modified basalt flake fiber pattern of example 2;
FIG. 5 is an infrared spectrum of a modified basalt flake fiber pattern of comparative test 2.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the surface treatment method of basalt scale fibers of the embodiment is carried out according to the following steps:
Firstly, adding a silane coupling agent into alcohol according to the mass percentage concentration of the silane coupling agent of 1-5% to obtain an alcohol solution of the silane coupling agent;
Secondly, adding basalt flake fibers into a coupling agent alcoholic solution to obtain a mixed solution; placing the mixed solution in a container, and carrying out high-speed shearing stirring for 20-60 min by using a high-speed shearing stirrer at the rotating speed of 1000-3000 rpm; then placing the mixture into an ultrasonic cleaning machine with the power of 300-700 w for ultrasonic dispersion for 20-60 min;
And thirdly, filtering the basalt scale fibers treated in the second step, washing with alcohol, drying the solvent, and standing at room temperature for 20-24 hours to complete the surface treatment of the basalt scale fibers.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the silane coupling agent in the step one is alkoxy silane containing amino, vinyl, sulfydryl, epoxy, cyano or methyl propionyl oxy; the rest is the same as the first embodiment.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the mass percentage concentration of the silane coupling agent in the first step is 2-4%; the other is the same as one of the first to second embodiments.
The fourth concrete implementation mode: the difference between the first embodiment and the third embodiment is that the rotation speed of the high-speed shearing mixer in the second step is 1200-2000 rpm; the others are the same as in one of the first to third embodiments.
the fifth concrete implementation mode: the difference between the embodiment and one of the first to fourth embodiments is that the high-speed shearing and stirring time in the second step is 30-50 min; the other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between the present embodiment and one of the first to fifth embodiments is that the power of the ultrasonic cleaner in the second step is 400-600 w; the other is the same as one of the first to fifth embodiments.
the seventh embodiment: the difference between the present embodiment and the first to sixth embodiments is that the dispersion time of the ultrasonic cleaner in the second step is 30-50 min; the other is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the first embodiment and the first to seventh embodiments is that the alcohol in the first step is one or a combination of two of methanol and ethanol; the other is the same as one of the first to seventh embodiments.
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: the surface treatment method of basalt scale fibers of the embodiment is carried out according to the following steps:
firstly, adding a silane coupling agent KH550 into ethanol according to the mass percentage concentration of the silane coupling agent KH550 of 1 percent to obtain an alcoholic solution of the silane coupling agent KH 550;
secondly, adding 5g of basalt scale fibers into 100g of KH550 alcohol solution serving as a coupling agent to obtain a mixed solution; placing the mixed solution in a beaker, and carrying out high-speed shearing and stirring for 20min by using a high-speed shearing stirrer under the condition that the rotating speed is 2000 rpm; then dispersing for 20min in an ultrasonic cleaning machine with the power of 500 w;
And thirdly, filtering the basalt flake fibers treated in the second step, washing with ethanol for 3 times, drying, and standing at 25 ℃ for 24 hours to allow the silane coupling agent to have enough time to contact with moisture in the air, thereby finishing the surface treatment of the basalt flake fibers.
Comparative experiment 1: the experiment differs from example 1 in that the following procedure is used in step two: adding 5g of basalt flake fibers into 100g of KH550 alcohol solution serving as a coupling agent to obtain a mixed solution, and stirring the mixed solution by using an electric stirrer at a low speed of 50rpm for 40 min; the other operations were the same as in example 1.
The infrared characterization of the unmodified basalt scale fibers, the modified basalt scale fibers of the example 1 and the basalt scale fibers treated in the comparative experiment 1 was performed by using a fourier infrared spectrometer, and the test results are shown in fig. 1, fig. 2 and fig. 3.
As can be seen by comparing FIG. 1 and FIG. 2, after the basalt scale fiber is modified in the embodiment 1, a plurality of dispersed peaks appear at the position of 3300-3500cm -1, which indicates that the surface of the basalt scale fiber is grafted with aminopropyl functional groups, and the double peaks at the positions of 1074-960 cm -1 are typical silicon-oxygen bond peak types, which proves that the silane coupling agent is successfully grafted on the surface of the fiber, and the infrared test result proves the modification effect of the embodiment.
as can be seen by comparing FIG. 2 with FIG. 3, the comparative test 1 has no high-speed shearing and ultrasonic oscillation treatment, and after alcohol washing and drying, the dispersion peak of amino group in the infrared spectrum does not appear, and only has a weak methylene vibration peak at 2923cm -1, which indicates that the coupling agent is not grafted on the fiber surface or has little content.
Example 2: the surface treatment method of basalt scale fibers of the embodiment is carried out according to the following steps:
Firstly, adding a silane coupling agent KH560 into ethanol according to the mass percentage concentration of the silane coupling agent KH560 of 5% to obtain a silane coupling agent KH560 alcoholic solution;
secondly, adding 5g of basalt scale fibers into 100g of a coupling agent KH560 alcoholic solution to obtain a mixed solution; shearing and stirring the mixed solution at a high speed for 30min by using a high-speed shearing stirrer under the condition that the rotating speed is 2000 rpm; then dispersing for 30min in an ultrasonic cleaning machine with the power of 500 w;
and thirdly, filtering the basalt flake fibers treated in the second step, sequentially washing the basalt flake fibers with ethanol for 3 times, washing the basalt flake fibers with water for 3 times, drying the basalt flake fibers, and placing the basalt flake fibers at the room temperature of 20 ℃ for 24 hours to enable the silane coupling agent to have enough time to contact with moisture in the air, so that the surface treatment of the basalt flake fibers is completed.
Comparative experiment 2: the experiment differs from example 2 in that the following procedure was used in step two: adding 5g of basalt flake fibers into 100g of coupling agent KH560 alcoholic solution to obtain a mixed solution, and stirring for 60min at a low speed of 100rpm by using a stirrer; the other operations were the same as in example 2.
The infrared spectrum of the basalt fiber modified in example 2 is shown in fig. 4, and the infrared spectrum of the basalt fiber modified in comparative test 2 is shown in fig. 5. comparing fig. 1 and fig. 4, it can be seen that alkyl C-H stretching vibration peaks at 2947cm -1 and 2842cm -1, carbonyl group stretching vibration peaks at 1718cm -1, and epoxy group characteristic peaks of KH-560 coupling agent at 940cm -1 appear on the infrared spectrum of the basalt fiber modified in this example, and it is proved that the surface treatment process of this example is feasible.
As can be seen by comparing FIG. 4 and FIG. 5, the infrared spectrum of the modified product of comparative experiment 2, which has not been subjected to the high-speed shearing and ultrasonic oscillation treatment, is substantially not different from that of the unmodified basalt fiber, and the circular peak at 3400cm -1 is attributed to slight water absorption after drying, which indicates that the process conditions of comparative experiment 2 are insufficient to complete the surface modification.
Claims (8)
1. A surface treatment method of basalt scale fibers is characterized by comprising the following steps:
Firstly, adding a silane coupling agent into alcohol according to the mass percentage concentration of the silane coupling agent of 1-5% to obtain an alcohol solution of the silane coupling agent;
Secondly, adding basalt flake fibers into a coupling agent alcoholic solution to obtain a mixed solution; placing the mixed solution in a container, and carrying out high-speed shearing stirring for 20-60 min by using a high-speed shearing stirrer at the rotating speed of 1000-3000 rpm; then placing the mixture into an ultrasonic cleaning machine with the power of 300-700 w for ultrasonic dispersion for 20-60 min;
And thirdly, filtering the basalt scale fibers treated in the second step, washing with alcohol, drying the solvent, and standing at room temperature for 20-24 hours to complete the surface treatment of the basalt scale fibers.
2. The method for surface treatment of basalt flake fiber according to claim 1, wherein the silane coupling agent in the first step is an alkoxysilane containing an amino group, a vinyl group, a mercapto group, an epoxy group, a cyano group and/or a methylpropanoyloxy group.
3. The surface treatment method of basalt flake fiber according to claim 1 or 2, characterized in that the mass percentage concentration of the silane coupling agent in the step one is 2% to 4%.
4. the surface treatment method of basalt flake fiber according to claim 1 or 2, characterized in that the rotation speed of the high speed shearing mixer in the second step is 1200 to 2000 rpm.
5. The surface treatment method of basalt flake fibers according to claim 1 or 2, characterized in that the high-speed shearing stirring time in the second step is 30 to 50 min.
6. The surface treatment method of basalt flake fibers according to claim 1 or 2, characterized in that the power of the ultrasonic cleaner in the second step is 400 to 600 w.
7. The surface treatment method of basalt flake fibers according to claim 1 or 2, characterized in that the dispersion time of the ultrasonic cleaner in the second step is 30 to 50 min.
8. The surface treatment method of basalt flake fiber according to claim 1 or 2, characterized in that the alcohol in the step one is one or a combination of two of methanol and ethanol.
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| CN201910973384.8A CN110550870A (en) | 2019-10-14 | 2019-10-14 | surface treatment method of basalt scale fibers |
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Cited By (3)
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| CN114591677A (en) * | 2022-03-31 | 2022-06-07 | 陕西科技大学 | Basalt nanosheet-based super-hydrophobic coating material and preparation method thereof |
| CN114790302A (en) * | 2022-04-12 | 2022-07-26 | 安徽鼎奂节能科技有限公司 | Sound-insulation, shock-absorption and heat-insulation polyurethane composite board |
| CN116285478A (en) * | 2023-04-03 | 2023-06-23 | 重庆智笃新材料科技有限公司 | Basalt inorganic long crystal flake fireproof paint and preparation method thereof |
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