CN111153608B - Organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and preparation method thereof - Google Patents
Organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and preparation method thereof Download PDFInfo
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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
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- C03C25/47—Coatings containing composite materials containing particles, fibres or flakes, e.g. in a continuous phase
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- 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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- 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
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Abstract
The invention discloses an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and a preparation method thereof, wherein the impregnating compound is prepared from the following components in percentage by mass: methyl phenyl silicone resin emulsion: 15 to 28 percent; low-temperature melting of glass powder: 10 to 20 percent; talc powder: 3 to 5 percent; mica powder: 1 to 4 percent; coupling agent KH-550:0.5-1%; sodium bentonite: 0.2-1%; water: and (4) the balance. The implementation of the coating modification technology achieves the purposes of improving the high temperature resistance, the bundling property and the wear resistance of the basalt fiber and softening the fiber, thereby improving the mechanical property and the high-temperature interface property of the basalt fiber material.
Description
Technical Field
The invention belongs to the technical field of impregnating compounds, relates to a basalt fiber impregnating compound, and particularly relates to an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and a preparation method thereof.
Background
Basalt fiber is a novel inorganic fiber, has a series of advantages of high strength, high temperature resistance, corrosion resistance and the like, but the characteristics of inorganic materials also enable the basalt fiber to have the defects of large brittleness and easy damage in the production and use processes compared with the traditional organic fiber. The basalt fiber has a unique physical structure and chemical composition, so that the basalt fiber is superior to glass fiber and chemical fiber in many technical indexes such as high temperature resistance (continuous temperature resistance of about 300-500 ℃), stability, corrosion resistance, hydrolysis resistance, insulativity and the like, and becomes an ideal high-temperature-resistant inorganic fiber.
It is known that sizing agents should be matched to the type and application of the fiber, which determines the performance properties of the fiber and its performance in composites. The film forming agent of the impregnating compound is the most important component in the impregnating compound formula. The importance of impregnating compounds is equivalent to the "chip manufacturing technology" of the IT industry. Generally, each product of a fiber manufacturer has a unique formula, and particularly, for brittle fibers, the size is more critical to the preparation and application of the fibers. Although China already masters the manufacturing technology of basalt fibers, the research and development of the special impregnating compound for the basalt fibers is still blank, and various manufacturers mostly apply the glass fiber impregnating compound to the basalt fibers.
The types of the film forming agents of the basalt fiber impregnating compound commonly used at present are as follows: epoxy resins, polyvinyl acetate (PVAc), polyesters, polyurethanes, polyacrylates, and the like. The existing basalt fiber impregnating compound has certain limitation in practical application, one film forming agent is poor in film forming performance when being used alone, and the phenomena of silk flying and hairiness are easily caused in subsequent processing. Chinese invention patent (CN 201510370194.9) discloses a water-based basalt fiber impregnating compound, which contains 46-62% of epoxy polymer emulsion, 8-12% of coupling agent and 1-2% of antistatic agent, and can improve the mechanical property and the bunching property of basalt fibers. Chinese invention patent (CN 201510981456.5) discloses a water-based basalt fiber impregnating compound, which contains 2-10% of water-soluble epoxy resin, 1-8% of polyvinyl alcohol, 0.5-1% of coupling agent, 0.2-0.8% of antistatic agent and 0.08-0.25% of pH regulator, and has good adhesion and film forming property. Chinese invention patent (CN 201510980061.3) discloses a water-based basalt fiber impregnating compound, which contains 3-8% of water-soluble epoxy resin, 2-6% of polyvinyl acetate emulsion, 0.5-1% of coupling agent, 0.2-0.8% of antistatic agent, 0.6-1.2% of plasticizer and 0.08-0.20% of pH regulator, and has good adhesion and film forming performance on basalt fibers. Chinese invention patent (CN 20160547303.4) discloses a wetting agent for fine denier boron oxide fiber and a preparation method thereof, wherein the wetting agent is prepared from n-dodecane, ethyl orthosilicate and polyether modified silicone antistatic agent. The impregnating compound is coated on the surface of a precursor boron oxide fiber, so that on one hand, a compact protective film can be formed on the surface of the boron oxide fiber, the fiber can be protected, and the strength of the boron oxide fiber can be improved; on the other hand, the antistatic property of the fine denier boron oxide fiber can be improved, the broken filaments of the fiber broken filaments are reduced, and the strength of the boron oxide fiber is improved. Chinese invention patent (CN 201710637728.9) discloses a special impregnating compound for aluminum oxide continuous fiber twisted yarn and a preparation method thereof, wherein the impregnating compound comprises the following components in percentage by weight: 3 to 6 percent of water-based epoxy emulsion, 0.2 to 0.6 percent of lubricant, 0.1 to 0.2 percent of antistatic agent, 0.3 to 0.8 percent of organosilane coupling agent, 0.02 to 0.05 percent of pH value regulator and the balance of water. The sizing agent of the invention endows the alumina continuous fiber with excellent flexibility, bundling property and lubricity, and protects the alumina continuous fiber from losing mechanical properties. The Chinese invention patent (CN 201810974812.4) discloses a glass fiber impregnating compound, which comprises a coupling agent, a lubricant, polyvinyl acetate emulsion, epoxy emulsion, a cross-linking agent, a pH value regulator and water. The content of each component is expressed by mass percent as follows: 0.1 to 0.5 percent of coupling agent, 0.1 to 0.5 percent of lubricant, 2.0 to 12.0 percent of polyvinyl acetate emulsion, 1.0 to 6.0 percent of epoxy emulsion, 0.05 to 0.5 percent of cross-linking agent, 0.05 to 0.5 percent of pH value regulator and 80.0 to 96.7 percent of water. The glass fiber yarn produced by using the impregnating compound can improve the color and the breaking strength of the yarn, can also effectively improve the fluidity of the glass fiber and improve the compatibility of the glass fiber with matrix resin. The Chinese invention patent (CN 201811097845.1) discloses a preparation method of an anti-corrosion glass fiber impregnating compound, namely, 20-30 parts of vinyl resin, 8-10 parts of compound emulsifier, 3-5 parts of linoleic acid and 60-80 parts of water are stirred to obtain No. 1 mixed slurry; heating and stirring 5-8 parts of modified nano metal powder, 8-10 parts of low-melting-point alloy, 10-20 parts of tetraethoxysilane, 20-30 parts of alcohol, 20-30 parts of acid and 5-8 parts of modified sepiolite to obtain No. 2 mixed slurry; finally, slurry No. 2 and slurry No. 1 were mixed according to the ratio of 1:5-1:10, stirring and mixing to prepare the corrosion-resistant glass fiber impregnating compound.
The film forming agent of the impregnating compound belongs to resin materials, and an organic film layer formed on the surface of the basalt fiber has poor temperature resistance. When the basalt fiber is used at high temperature (not less than 300 ℃), an organic film layer formed by the impregnating compound is thermally decomposed, the function of the impregnating compound is lost, and the high-temperature performance advantage of the basalt fiber is seriously influenced.
Disclosure of Invention
The invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and a preparation method thereof, which aim to overcome the defects of the prior art.
In order to achieve the aim, the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound which is prepared from the following components in percentage by mass: methyl phenyl silicone resin emulsion: 15 to 28 percent; low-temperature melting of glass powder: 10 to 20 percent; talc powder: 3 to 5 percent; mica powder: 1 to 4 percent; coupling agent KH-550:0.5 to 1 percent; sodium bentonite: 0.2-1%; water: and the balance.
Further, the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound, which also has the following characteristics: wherein the low-temperature melting glass powder is formed by mixing 400 ℃, 450 ℃, 500 ℃ and 580 ℃ low-temperature melting glass powder; the mass ratio of the 400 ℃ low-temperature melting glass powder, the 450 ℃ low-temperature melting glass powder, the 500 ℃ low-temperature melting glass powder and the 580 ℃ low-temperature melting glass powder is 4: 3: 2: 1.
Further, the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound, which also has the following characteristics: wherein the size of the low-temperature melting glass powder is 100-500mm.
Further, the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound, which also has the following characteristics: wherein the low-temperature melting glass powder is lead-free low-temperature melting glass powder.
Further, the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound, which also has the following characteristics: wherein, the solid phase content in the methyl phenyl organic silicon resin emulsion is 40-55%.
The invention also provides a preparation method of the organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound, according to the formula, firstly adding the coupling agent KH-550, sodium bentonite, low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering; and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
The impregnating compound is applied to basalt fibers with the working temperature of more than 400 ℃.
The invention has the beneficial effects that: the invention provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound and a preparation method thereof. When the sizing agent is coated, the low-temperature molten glass powder and the methyl phenyl organic silicon resin form a microcapsule structure which takes organic silicon as a capsule and takes the low-temperature molten glass powder as a core. The microcapsules are stably and uniformly dispersed in the organic silicon resin matrix under the action of various fillers and coupling agents. And the organic silicon in-situ polymerization film layer formed on the surface of the basalt fiber is wrapped with microcapsules of low-temperature molten glass micro powder with different melting temperatures. When the basalt fiber works at the working temperature of more than 400 ℃ for a long time, part of organic silicon (including capsules and a matrix) is decomposed into silicon oxide inorganic phases, so that the volume shrinkage capsules crack, at the moment, low-temperature molten glass powder which is molten at the temperature overflows from the cracks to fill the cracks, the glass powder is a complex oxide containing aluminum oxide, silicon oxide and the like and reacts with silicon oxide which is newly generated by the decomposition of the organic silicon and has high activity to form an oxide crystal phase, and therefore the repairing effect on the crack of the fiber surface coating (the matrix and the microcapsules) is achieved. And in a high-temperature service state, the low-temperature molten glass micro powder is changed into a viscous state, and the overflowing, filling and repairing capabilities are kept at any time.
When the working temperature reaches the melting point of a certain type of glass powder, the part of glass powder is melted, the rest of glass powder is still in a solid state, the stability of the microcapsule and the matrix can be ensured by the part of glass powder in the solid state, and the instability of the integral coating on the fiber caused by the full liquid state is avoided. The highest working temperature of the basalt fiber is usually not more than 550 ℃, and the glass powder composition with a plurality of gradually increased melting points can be suitable for various working temperatures.
The invention provides a microcapsule type high-temperature self-repairing organic-inorganic hybrid basalt fiber water-based impregnating compound which is a special impregnating compound suitable for exerting the high-temperature use performance of basalt fibers and can form a microcapsule type high-temperature self-repairing organic-inorganic hybrid film on the surfaces of the basalt fibers. The technology of the invention is suitable for basalt fiber braided fabrics applied at high temperature. The coating can resist high temperature (more than or equal to 400 ℃), and the technical problems that a special impregnating compound for basalt fibers is lacked and the impregnating compound is not high in temperature resistance and is easy to decompose at present are solved.
By implementing the novel impregnating compound technology, the high temperature resistance, the bundling property and the wear resistance of the basalt fiber can be improved, and the softening effect is exerted on the fiber, so that the mechanical property of the basalt fiber is improved, and the purpose of improving the high-temperature interface property of the basalt fiber material is achieved. The high-quality impregnating compound is provided for improving the technical level of basalt fiber preparation in China, and technical support is provided for popularization and application of basalt fiber composite materials.
Drawings
Fig. 1 is an SEM image of basalt fiber coated with the impregnating compound of example 1.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The embodiment provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound which is prepared from the following components in parts by weight:
methyl phenyl silicone resin emulsion (solid content 50%): 28%;
environment-friendly low-temperature molten glass powder (100-500 mm): 20 percent;
talc powder: 5 percent;
mica powder: 4 percent;
coupling agent KH-550:1 percent;
sodium bentonite: 1 percent;
water: and (4) the balance.
Wherein the environment-friendly low-temperature melting glass powder is formed by mixing 400 ℃ low-temperature melting glass powder, 450 ℃ low-temperature melting glass powder, 500 ℃ low-temperature melting glass powder and 580 ℃ low-temperature melting glass powder according to the mass ratio of 4: 3: 2: 1.
The preparation method of the organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound comprises the following steps: according to the formula, firstly adding a coupling agent KH-550, sodium bentonite, environment-friendly low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering; and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
As shown in figure 1, the surface of the basalt fiber coated with the impregnating compound is covered by a continuous organic-inorganic hybrid film forming and microcapsule high-temperature self-repairing film, and a small amount of micron-sized low-melting glass powder overflowing granular attachments are arranged on the film. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.02 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
The basalt fiber treated by the basalt fiber impregnating compound of the current commercial mainstream aqueous epoxy film-forming agent has the thermal weight loss of more than 1% at 550 ℃ and the tensile strength of the fiber of less than 0.5N/tex.
Example 2
The embodiment provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound which is prepared from the following components in parts by weight:
methyl phenyl silicone resin emulsion (solid content 55%): 15 percent;
environment-friendly low-temperature molten glass powder (100-500 mm): 10 percent;
talc powder: 3 percent;
mica powder: 1 percent;
coupling agent KH-550:0.5 percent;
sodium bentonite: 0.2 percent;
water: and the balance.
Wherein the environment-friendly low-temperature melting glass powder is formed by mixing 400 ℃ low-temperature melting glass powder, 450 ℃ low-temperature melting glass powder, 500 ℃ low-temperature melting glass powder and 580 ℃ low-temperature melting glass powder according to the mass ratio of 4: 3: 2: 1.
The preparation method of the organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound comprises the following steps: according to the formula, firstly adding a coupling agent KH-550, sodium bentonite, environment-friendly low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering; and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a continuous organic-inorganic hybrid film and a microcapsule high-temperature self-repairing film, and a small amount of granular attachments overflowing from micron-sized low-melting glass powder are also arranged on the film. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.01 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
Example 3
The embodiment provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound which is prepared from the following components in parts by weight:
methyl phenyl silicone resin emulsion (solid content 40%): 25 percent;
environment-friendly low-temperature molten glass powder (100-500 mm): 15 percent;
talc powder: 4 percent;
mica powder: 3 percent;
coupling agent KH-550:1 percent;
sodium bentonite: 0.8 percent;
water: and (4) the balance.
Wherein the environment-friendly low-temperature melting glass powder is formed by mixing 400 ℃ low-temperature melting glass powder, 450 ℃ low-temperature melting glass powder, 500 ℃ low-temperature melting glass powder and 580 ℃ low-temperature melting glass powder according to the mass ratio of 4: 3: 2: 1.
The preparation method of the organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound comprises the following steps: according to the formula, firstly, adding a coupling agent KH-550, sodium bentonite, environment-friendly low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering; and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a continuous organic-inorganic hybrid film forming and microcapsule high-temperature self-repairing film, and a small amount of micron-sized granular attachments overflowing from low-melting glass powder are arranged on the film. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.02%, and the tensile strength of the fiber is higher than 0.5N/tex.
Example 4
The embodiment provides an organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound which is prepared from the following components in parts by weight:
methyl phenyl silicone resin emulsion (solid content 52%): 28%;
environment-friendly low-temperature molten glass powder (100-500 mm): 14 percent;
talc powder: 5 percent;
mica powder: 3 percent;
coupling agent KH-550:1 percent;
sodium bentonite: 1 percent;
water: and (4) the balance.
Wherein the environment-friendly low-temperature melting glass powder is formed by mixing 400 ℃ low-temperature melting glass powder, 450 ℃ low-temperature melting glass powder, 500 ℃ low-temperature melting glass powder and 580 ℃ low-temperature melting glass powder according to the mass ratio of 4: 3: 2: 1.
The preparation method of the organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound comprises the following steps: according to the formula, firstly adding a coupling agent KH-550, sodium bentonite, environment-friendly low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering; and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a continuous organic-inorganic hybrid film and a microcapsule high-temperature self-repairing film, and a small amount of granular attachments overflowing from micron-sized low-melting glass powder are also arranged on the film. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.01 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
Claims (5)
1. An organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound is characterized in that:
the composition is prepared from the following components in percentage by mass:
methyl phenyl silicone resin emulsion: 15 to 28 percent;
low-temperature melting of glass powder: 10 to 20 percent;
talc powder: 3 to 5 percent;
mica powder: 1 to 4 percent;
coupling agent KH-550:0.5 to 1 percent;
sodium bentonite: 0.2 to 1 percent;
water: the balance;
wherein the low-temperature melting glass powder is formed by mixing 400 ℃ low-temperature melting glass powder, 450 ℃ low-temperature melting glass powder, 500 ℃ low-temperature melting glass powder and 580 ℃ low-temperature melting glass powder;
the mass ratio of the 400 ℃ low-temperature melting glass powder, the 450 ℃ low-temperature melting glass powder, the 500 ℃ low-temperature melting glass powder and the 580 ℃ low-temperature melting glass powder is 4: 3: 2: 1.
2. The organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound according to claim 1, which is characterized in that:
wherein the size of the low-temperature melting glass powder is 100-500mm.
3. The organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound according to claim 1, which is characterized in that:
wherein the low-temperature molten glass powder is lead-free low-temperature molten glass powder.
4. The organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound according to claim 1, which is characterized in that:
wherein the solid phase content of the methyl phenyl organic silicon resin emulsion is 40-55%.
5. The organic-inorganic hybrid film-forming microcapsule type high-temperature self-repairing basalt fiber water-based impregnating compound according to claim 1, wherein:
according to the formula, firstly, adding the coupling agent KH-550, sodium bentonite, low-temperature molten glass powder, talcum powder and mica powder into water while stirring, grinding for 2 hours by using a sand mill, and filtering;
and finally, adding the methyl phenyl organic silicon resin emulsion under low-speed stirring, and uniformly stirring to obtain the finished impregnating compound.
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