CN111204996A - Silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound and preparation method thereof - Google Patents
Silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound and preparation method thereof Download PDFInfo
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- CN111204996A CN111204996A CN202010052359.9A CN202010052359A CN111204996A CN 111204996 A CN111204996 A CN 111204996A CN 202010052359 A CN202010052359 A CN 202010052359A CN 111204996 A CN111204996 A CN 111204996A
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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
- C03C25/465—Coatings containing composite materials
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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
- C03C25/42—Coatings containing inorganic materials
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Abstract
The invention discloses a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound and a preparation method thereof, wherein the impregnating compound is prepared from the following components in percentage by mass: silicone-acrylic emulsion: 15 to 25 percent; magnesium oxide: 20 to 30 percent; magnesium chloride hexahydrate: 6 to 10 percent; magnesium sulfate heptahydrate: 3 to 5 percent; polyvinylpyrrolidone: 1 to 2 percent; coupling agent: 0.5-1%; water: and (4) the balance. The impregnating compound is coated on basalt fibers, and the obtained silicon-magnesium-based composite film is uniform in adhesion, high in film strength and good in toughness. The basalt fiber treated by the impregnating compound has improved high temperature resistance, bundling property, wear resistance and softening function, and is suitable for long-term use at the temperature of more than 300 ℃.
Description
Technical Field
The invention belongs to the technical field of impregnating compounds, relates to a basalt fiber impregnating compound, and particularly relates to a silicon-magnesium-based high-temperature-resistant basalt fiber 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 use of the fiber, which determines the performance of the fiber and its performance in composites. The film forming agent of the impregnating compound is the most important component in the formulation of the impregnating compound. The importance of the impregnating compound 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 still falls into the 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 (CN201510370194.9) discloses a water-based basalt fiber impregnating compound, which contains 46-62% of epoxy polymerization emulsion, 8-12% of coupling agent and 1-2% of antistatic agent, and can improve the mechanical property and the bunching property of basalt fiber. Chinese invention patent (CN201510981456.5) 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 (CN201510980061.3) 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 property for basalt fiber. The Chinese invention patent (CN20160547303.4) discloses a treating compound for fine denier boron oxide fiber and a preparation method thereof, wherein the treating compound is prepared from n-dodecane, ethyl orthosilicate and polyether modified organosilicon antistatic agent. The sizing agent is coated on the surface of the boron oxide fiber of the precursor, so that on one hand, a layer of 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 (CN201710637728.9) discloses a special impregnating compound for twisted yarns of alumina continuous fibers and a preparation method thereof, wherein the impregnating compound comprises the following components in percentage by weight: 3-6% of water-based epoxy emulsion, 0.2-0.6% of lubricant, 0.1-0.2% of antistatic agent, 0.3-0.8% of organosilane coupling agent, 0.02-0.05% 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 (CN201810974812.4) 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: 0.1-0.5% of coupling agent, 0.1-0.5% of lubricant, 2.0-12.0% of polyvinyl acetate emulsion, 1.0-6.0% of epoxy emulsion, 0.05-0.5% of cross-linking agent, 0.05-0.5% of pH value regulator and 80.0-96.7% of water. The glass fiber yarn produced by using the impregnating compound can improve the color and the breaking strength of the yarn, effectively improve the fluidity of the glass fiber and improve the compatibility of the glass fiber yarn and matrix resin. The Chinese invention patent (CN201811097845.1) 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 ethyl orthosilicate, 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 nos. 2 and 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 the temperature resistance of an organic film layer formed on the surface of basalt fiber is poor. 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 a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound and a preparation method thereof, which are used for overcoming the defects of the prior art.
In order to achieve the aim, the invention provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound which is prepared from the following components in percentage by mass: silicone-acrylic emulsion: 15 to 25 percent; magnesium oxide: 20 to 30 percent; magnesium chloride hexahydrate: 6 to 10 percent; magnesium sulfate heptahydrate: 3 to 5 percent; polyvinylpyrrolidone: 1 to 2 percent; coupling agent: 0.5-1%; water: and (4) the balance.
Further, the invention provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound, which can also have the following characteristics: wherein the magnesium oxide is light-burned magnesium oxide.
Further, the invention provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound, which can also have the following characteristics: wherein, the solid content of the silicone-acrylate emulsion is 40-50%.
Further, the invention provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound, which can also have the following characteristics: wherein the coupling agent is a silane coupling agent KH 550.
The impregnating compound is applied to basalt fibers with the working temperature of more than 300 ℃.
The invention also provides a preparation method of the silicon-magnesium based high-temperature-resistant basalt fiber impregnating compound, which comprises the following steps of putting water into a reaction container according to a formula, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution; magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved; adding magnesium oxide into a reaction container and stirring to obtain colloidal liquid with certain viscosity; slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
The invention has the beneficial effects that: the invention provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound and a preparation method thereof, wherein the impregnating compound is silicon-acrylic emulsionThe liquid, magnesium oxide, magnesium chloride hexahydrate, magnesium sulfate heptahydrate, polyvinylpyrrolidone, a coupling agent and water. In the preparation process, the magnesium oxide is hydrated to generate Mg (OH) under the action of magnesium chloride hexahydrate, magnesium sulfate heptahydrate and water2And the magnesium gel particle product. Then under the coupling and dispersing action of the coupling agent and the polyvinylpyrrolidone, the magnesium gel particles are uniformly dispersed in the silicone-acrylic emulsion to form a water-based impregnating compound solution. In the coating process, Mg (OH)2And the magnesium gel particles and the silicone-acrylate emulsion form a uniform and compact inorganic-organic hybrid film on the surface of the basalt fiber, so that the basalt fiber is infiltrated and protected. When the basalt fiber treated by the impregnating compound is used at a temperature of more than 300 ℃ or even higher for a long time, the organosilicon component in the cured product of the silicone-acrylic emulsion in the inorganic-organic hybrid film is decomposed into silicon oxide, and Mg (OH)2Etc. the gel material also decomposes to produce magnesium oxide. The silicon oxide and magnesium oxide generated by these new decompositions have relatively high chemical activity. Under high temperature, the high chemical activity silicon oxide and magnesium oxide and the components of silicon oxide, aluminum oxide, iron oxide and the like contained in the basalt fiber can generate complex chemical interaction, and further a uniform, continuous and high-stability thin layer of silicon oxide and magnesium oxide is formed on the surface of the basalt fiber.
Among them, the magnesium oxide is preferably light-burned magnesium oxide, and has higher activity. Polyvinylpyrrolidone and coupling agent, during the preparation process, the Mg (OH) formed can be used2The magnesium gel particles are better dispersed in the silicone-acrylic emulsion; in the coating process, the water-based impregnating compound solution can better form a film on the surface of the basalt fiber.
The invention provides a silicon-magnesium-based composite film type basalt fiber water-based impregnating compound, which is characterized in that a silicon-magnesium oxide-based composite inorganic film is formed on the surface of basalt fiber, and the silicon-magnesium oxide-based composite inorganic film on the surface of the basalt fiber is not decomposed and degraded at the working temperature of more than 300 ℃, so that the technical problems that the impregnating compound special for basalt fiber is lacked and the impregnating compound is not high in temperature resistance and is easy to decompose at present are solved.
By implementing the coating modification technology, the high temperature resistance, the bundling property and the wear resistance of the basalt fiber can be improved, the softening effect on the fiber is realized, the mechanical property of the basalt fiber is further improved, the purpose of improving the high-temperature interface property of the basalt fiber material is achieved, and the basalt fiber braided fabric is suitable for high-temperature application. 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 a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound which is prepared from the following components in percentage by mass:
silicone-acrylic emulsion (solid content 40%): 25 percent;
light-burned magnesium oxide: 30 percent;
magnesium chloride hexahydrate: 10 percent;
magnesium sulfate heptahydrate: 5 percent;
polyvinylpyrrolidone: 2 percent;
silane coupling agent KH 550: 1 percent;
water: and (4) the balance.
The preparation method of the silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound comprises the following steps: according to the formula, putting water into a reaction vessel, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution; magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved; adding light-burned magnesium oxide into a reaction container and stirring to obtain colloidal liquid with certain viscosity; slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
As shown in figure 1, the surface of the basalt fiber coated by the impregnating compound is covered by a uniform and continuous silicon magnesium oxide composite inorganic film, and a small amount of micron-sized granular attachments are also arranged on the film layer. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.08%, and the tensile strength of the fiber is higher than 0.5N/tex.
The thermal weight loss of the basalt fiber treated by the basalt fiber impregnating compound adopting the current commercial mainstream aqueous epoxy film forming agent at 550 ℃ is more than 1 percent, and the tensile strength of the fiber is lower than 0.5N/tex.
Example 2
The embodiment provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound which is prepared from the following components in percentage by mass:
silicone-acrylic emulsion (solid content 50%): 15 percent;
light-burned magnesium oxide: 20 percent;
magnesium chloride hexahydrate: 6 percent;
magnesium sulfate heptahydrate: 3 percent;
polyvinylpyrrolidone: 1 percent;
silane coupling agent KH 550: 0.5 percent;
water: and (4) the balance.
The preparation method of the silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound comprises the following steps: according to the formula, putting water into a reaction vessel, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution; magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved; adding light-burned magnesium oxide into a reaction container and stirring to obtain colloidal liquid with certain viscosity; slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a uniform and continuous silicon magnesium oxide composite inorganic film, and a small amount of micron-sized granular attachments are also arranged on the film layer. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.05 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
Example 3
The embodiment provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound which is prepared from the following components in percentage by mass:
silicone-acrylic emulsion (solids content 42%): 20 percent;
light-burned magnesium oxide: 25 percent;
magnesium chloride hexahydrate: 8 percent;
magnesium sulfate heptahydrate: 4 percent;
polyvinylpyrrolidone: 1.5 percent;
silane coupling agent KH 550: 0.8 percent;
water: and (4) the balance.
The preparation method of the silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound comprises the following steps: according to the formula, putting water into a reaction vessel, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution; magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved; adding light-burned magnesium oxide into a reaction container and stirring to obtain colloidal liquid with certain viscosity; slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a uniform and continuous silicon magnesium oxide composite inorganic film, and a small amount of micron-sized granular attachments are also arranged on the film layer. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.06 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
Example 4
The embodiment provides a silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound which is prepared from the following components in percentage by mass:
silicone-acrylic emulsion (solids content 42%): 15 percent;
light-burned magnesium oxide: 30 percent;
magnesium chloride hexahydrate: 10 percent;
magnesium sulfate heptahydrate: 5 percent;
polyvinylpyrrolidone: 2 percent;
silane coupling agent KH 550: 1 percent;
water: and (4) the balance.
The preparation method of the silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound comprises the following steps: according to the formula, putting water into a reaction vessel, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution; magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved; adding light-burned magnesium oxide into a reaction container and stirring to obtain colloidal liquid with certain viscosity; slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
The surface of the basalt fiber coated by the impregnating compound is covered by a uniform and continuous silicon magnesium oxide composite inorganic film, and a small amount of micron-sized granular attachments are also arranged on the film layer. The thermal weight loss of the basalt fiber at 550 ℃ is less than 0.05 percent, and the tensile strength of the fiber is higher than 0.5N/tex.
Claims (5)
1. A silicon-magnesium-based high-temperature-resistant basalt fiber impregnating compound is characterized in that:
the composition is prepared from the following components in percentage by mass:
silicone-acrylic emulsion: 15 to 25 percent;
magnesium oxide: 20 to 30 percent;
magnesium chloride hexahydrate: 6 to 10 percent;
magnesium sulfate heptahydrate: 3 to 5 percent;
polyvinylpyrrolidone: 1 to 2 percent;
coupling agent: 0.5-1%;
water: and (4) the balance.
2. The silicon-magnesium based high temperature resistant basalt fiber impregnating compound according to claim 1, wherein:
wherein the magnesium oxide is light-burned magnesium oxide.
3. The silicon-magnesium based high temperature resistant basalt fiber impregnating compound according to claim 1, wherein:
wherein the solid content of the silicone-acrylic emulsion is 40-50%.
4. The silicon-magnesium based high temperature resistant basalt fiber impregnating compound according to claim 1, wherein:
wherein the coupling agent is a silane coupling agent KH 550.
5. The method for preparing the silicon-magnesium based high-temperature resistant basalt fiber impregnating compound according to claim 1, which is characterized in that:
according to the formula, putting water into a reaction vessel, heating to 80 ℃, adding magnesium chloride hexahydrate, and stirring to obtain a magnesium chloride solution;
magnesium sulfate heptahydrate is slowly added into the obtained magnesium chloride solution and stirred until the magnesium sulfate heptahydrate is completely dissolved;
adding magnesium oxide into the reaction container and stirring to obtain colloidal liquid;
slowly dripping the silicone-acrylic emulsion into a reaction container, adding polyvinylpyrrolidone and a coupling agent after dripping is finished, stirring, and cooling to room temperature to obtain the impregnating compound.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694739A (en) * | 2016-04-19 | 2016-06-22 | 中南林业科技大学 | Silicone acrylic emulsion modified magnesium-containing inorganic adhesive for straws and preparation method of silicone acrylic emulsion modified magnesium-containing inorganic adhesive |
| CN107619200A (en) * | 2017-10-17 | 2018-01-23 | 高昕文 | A kind of glass fiber infiltration agent and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694739A (en) * | 2016-04-19 | 2016-06-22 | 中南林业科技大学 | Silicone acrylic emulsion modified magnesium-containing inorganic adhesive for straws and preparation method of silicone acrylic emulsion modified magnesium-containing inorganic adhesive |
| CN107619200A (en) * | 2017-10-17 | 2018-01-23 | 高昕文 | A kind of glass fiber infiltration agent and preparation method thereof |
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