CN112126123A - Continuous basalt fiber surface treating agent and preparation method thereof - Google Patents
Continuous basalt fiber surface treating agent and preparation method thereof Download PDFInfo
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- CN112126123A CN112126123A CN202010856390.8A CN202010856390A CN112126123A CN 112126123 A CN112126123 A CN 112126123A CN 202010856390 A CN202010856390 A CN 202010856390A CN 112126123 A CN112126123 A CN 112126123A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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Abstract
The invention discloses a continuous basalt fiber surface treating agent and a preparation method thereof. According to the invention, polypropylene grafted maleic anhydride is used as an interface compatilizer, so that on one hand, MAH can perform esterification reaction with the surface of fiber to reduce the polarity of the fiber, and the MAH and the fiber are bonded together through chemical bonds; on the other hand, MAH can react with macromolecular free radicals in polypropylene groups to be embedded into the matrix, so that the fibers and the matrix are connected through PP-g-MAH to form strong interface combination. Meanwhile, the silane coupling agent is added to promote the affinity and the interface bonding force of PP and the fiber, improve the technological performance of the fiber and ensure that the performance conversion rate of the fiber and the performance of the composite material are at a higher level. The invention is mainly used in the field of interface modification of thermoplastic resin and basalt fiber, and can fully exert the excellent effect of the basalt fiber reinforced thermoplastic resin matrix composite material.
Description
Technical Field
The invention relates to a preparation method of a surface treating agent when continuous fibers are combined with thermoplastic resin, in particular to a surface treating agent between continuous basalt fibers and polypropylene resin and a preparation method thereof.
Background
The continuous fiber reinforced thermoplastic resin matrix composite material has the advantages of high performance, high forming speed, recoverability, cyclic utilization and the like, and the development is rapid in recent years. The basalt fiber is the fourth high-performance fiber after carbon fiber, aramid fiber and ultra-high molecular weight polyethylene fiber, and is one of the high and new technical fibers which are mainly developed in China. China is one of the main producing and applying countries of basalt fibers, however, at present, basalt fibers are mainly used for thermosetting resin-based composite materials in China, and no mature basalt fibers and composite material products suitable for thermoplastic resins exist. The thermoplastic resin has low polarity and reactivity, the wettability with the fiber is poor, and chemical bonding is difficult to form, so that the interface performance between the fiber and the resin is poor, the fiber performance is difficult to be efficiently converted into the performance of the composite material, and the application effect of the fiber and the composite material is severely limited. Compared with the glass fiber of the reinforced thermoplastic composite material which is widely applied at present, the basalt fiber has the advantages of mechanical property, corrosion resistance, low toxicity, flame retardant property, environmental protection and the like, and if the special basalt fiber which is suitable for thermoplastic resin can be developed, the application field of the basalt fiber can be greatly widened, and the performance advantages can be exerted. For the glass fiber, the corresponding fiber surface treatment technology and glass fiber products are provided for each thermoplastic resin matrix, and the interface performance of the glass fiber and the matrix is ensured. The composition and structure of the basalt fiber and the glass fiber are obviously different, so that the surface treatment technology of the glass fiber cannot be directly used for the basalt fiber or has poor direct use effect, and the development of the special surface treatment agent for the basalt fiber is necessary to improve the wettability and the reactivity of the basalt fiber and the thermoplastic resin, which is the core of the technology for developing the basalt fiber for the thermoplastic resin.
Disclosure of Invention
The invention aims to solve the technical problem of providing a continuous basalt fiber surface treating agent suitable for a polypropylene resin matrix composite material and a preparation method thereof, so as to overcome the problem of poor interface property of the existing thermoplastic resin and basalt fiber.
The continuous basalt fiber surface treating agent comprises 100 parts of deionized water, 5-10 parts of a film forming agent, 0.1-0.5 part of a lubricating agent, 0.2-1.0 part of a coupling agent and 0.1-0.5 part of an antistatic agent.
The film forming agent is polypropylene grafted maleic anhydride (PP-g-MAH), the grafting rate of the film forming agent is 0.5-2%, and the film forming agent contains 5-10% of an emulsifier, wherein the emulsifier is span-80 or sodium dodecyl sulfate and the like.
The coupling agent is one or a combination solution of more of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma-methacryloxypropyltrimethoxysilane (KH 570).
The lubricant is one or a mixed solution of more of cationic ammonia or modified silicone oil.
The antistatic agent is one or a mixture of more of quaternary ammonium salt and ammonium sulfonate.
A preparation method of a continuous basalt fiber surface treating agent comprises the following steps: adding 5-10 parts of film forming agent, 0.1-0.5 part of lubricant, 0.2-1.0 part of coupling agent and 0.1-0.5 part of antistatic agent into 100 parts of deionized water by weight, and uniformly stirring at the temperature of 18-25 ℃ to obtain the surface treating agent.
The continuous basalt fiber after surface treatment is prepared by using the surface treatment agent to perform surface treatment on the continuous basalt fiber.
The preparation method of the continuous basalt fiber subjected to surface treatment comprises the following steps: and (2) immersing the continuous basalt fiber into a liquid storage tank or a sizing roller in which the treating agent is placed under the action of a traction device, wherein the traction speed is 1-10 m/min, the content of the surface treating agent on the continuous basalt fiber can be adjusted through the change of the traction speed, and then drying for 30 min-3 h at the temperature of 80-140 ℃ to obtain the continuous basalt fiber subjected to surface treatment.
The linear density of the continuous basalt fibers is between 100 and 4800 tex.
A continuous basalt fiber reinforced polypropylene composite material is prepared from PP and the continuous basalt fiber subjected to surface treatment.
The preparation method of the continuous basalt fiber reinforced polypropylene composite material comprises the following steps: and (3) preparing PP and the continuous basalt fiber subjected to surface treatment into a prepreg at 160-200 ℃ by a hot melting method. The obtained prepreg is further used for preparing a composite material product by a mould pressing process or a vacuum bag process and the like.
In the composite material, the mass fraction of the continuous basalt fibers is between 40 and 70 percent.
The invention has the beneficial effects that: the surface treating agent disclosed by the invention has good wettability and reactivity on basalt fibers, effectively promotes affinity and interface binding force of polypropylene (PP) and basalt fibers, improves the technological properties of the fibers, and ensures that the performance conversion rate of the fibers and the performance of a composite material are at a higher level.
Drawings
The invention has the following drawings:
FIG. 1 is a schematic diagram of the polypropylene grafted maleic anhydride (PP-g-MAH) as an interfacial compatibilizer in the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
According to the continuous basalt fiber surface treating agent for the polypropylene-based composite material and the preparation method thereof, PP-g-MAH is used as an interface compatilizer, so that on one hand, the MAH can perform esterification reaction with the fiber surface to reduce the polarity of the fiber, and the MAH and the fiber surface are combined together through chemical bonds; on the other hand, MAH can react with macromolecular free radicals in polypropylene groups to be embedded into the matrix, so that the fibers and the matrix are connected through PP-g-MAH to form strong interfacial bonding, and FIG. 1 is a schematic diagram of the polypropylene grafted maleic anhydride (PP-g-MAH) as an interfacial compatilizer in the invention. Meanwhile, the silane coupling agent is added to promote the affinity and the interface bonding force of PP and the fiber, improve the technological performance of the fiber and ensure that the performance conversion rate of the fiber and the performance of the composite material are at a higher level.
The invention relates to a continuous basalt fiber surface treating agent for polypropylene-based composite materials and a preparation method thereof. Adding 5-10 parts of film forming agent, 0.1-0.5 part of lubricating agent, 0.2-1.0 part of coupling agent and 0.1-0.5 part of antistatic agent into 100 parts of deionized water by weight.
In the invention, the film-forming agent is polypropylene grafted maleic anhydride, the grafting ratio is between 0.5% and 2%, and the film-forming agent contains 5-10% of emulsifier, wherein the emulsifier is span-80, sodium dodecyl sulfate and the like.
In the invention, the coupling agent is one or a combination solution of a plurality of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma-methacryloxypropyltrimethoxysilane (KH 570).
In the invention, the lubricant is one or a mixed solution of more of cationic ammonia or modified silicone oil.
In the invention, the antistatic agent is a mixed solution of one or more of quaternary ammonium salt and ammonium sulfonate.
Example 1
The first step is as follows: preparation of surface treating agent
Adding 5 parts of film forming agent, 0.1 part of lubricating agent, 0.2 part of coupling agent and 0.1 part of antistatic agent into 100 parts of deionized water by weight, and uniformly stirring at the temperature of 20 ℃ to prepare the surface treating agent.
The film forming agent is polypropylene grafted maleic anhydride, the grafting rate of the film forming agent is 1%, and the film forming agent contains span-80 of 5%.
The lubricant is a product obtained by reacting nonanoic acid with tetra ethyl pentamine.
The coupling agent is gamma-aminopropyl triethoxysilane (KH 550).
The antistatic agent is tributyl methyl ammonium bis (trifluoromethyl) sulfonyl imide salt.
The second step is that: impregnated fiber
And (2) immersing the continuous basalt fiber into a liquid storage tank in which the surface treatment agent prepared in the first step is placed under the action of a traction device, wherein the traction speed is 2m/min, and then drying for 1h at the temperature of 80 ℃ to obtain the continuous basalt fiber subjected to surface treatment.
The linear density of the continuous basalt fibers is 1200 tex.
The third step: preparation of continuous basalt fiber reinforced polypropylene composite material
And (3) preparing PP and the basalt fiber subjected to surface treatment into a prepreg at 180 ℃ by using a hot press molding mode.
The basalt fiber is a continuous fiber, and the mass content of the fiber is 60%.
The mechanical properties of the polypropylene-based continuous basalt fiber composite material prepared in example 1 and the polypropylene-based continuous basalt fiber composite material prepared by preparing fibers with the general surface treatment agent are shown in the following table, and it can be seen that the properties of the composite material are obviously improved by using the surface treatment agent of the present invention.
Example 2
The first step is as follows: preparation of surface treating agent
Adding 10 parts of film forming agent, 0.5 part of lubricating agent, 1.0 part of coupling agent and 0.2 part of antistatic agent into 100 parts of deionized water by weight, and uniformly stirring at the temperature of 20 ℃.
The film forming agent is polypropylene grafted maleic anhydride, the grafting rate of the film forming agent is 2%, and the film forming agent contains 6% of emulsifier sodium dodecyl sulfate.
The lubricant is long-chain alkyl modified silicone oil.
The coupling agent is a combined solution of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma-methacryloxypropyltrimethoxysilane (KH 570).
The antistatic agent is 1-butyl-3-methylimidazole chlorine salt.
The second step is that: impregnated fiber
And (2) immersing the continuous basalt fiber on an applicator roll in which the surface treatment agent prepared in the first step is placed under the action of a traction device, wherein the traction speed is 5m/min, and then drying for 1h at the temperature of 80 ℃ to obtain the continuous basalt fiber with the surface treatment.
The linear density of the continuous basalt fibers is 1200 tex.
The third step: preparation of continuous basalt fiber reinforced polypropylene composite material
And (3) preparing PP and the basalt fiber subjected to surface treatment into a prepreg at 180 ℃ by using a hot press molding mode.
The basalt fiber is a continuous fiber, and the mass content of the fiber is 60%.
The mechanical properties of the polypropylene-based continuous basalt fiber composite material prepared in example 2 and the polypropylene-based continuous basalt fiber composite material prepared by preparing fibers with the general surface treatment agent are shown in the following table, and it can be seen that the properties of the composite material are obviously improved by using the surface treatment agent of the present invention.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the relevant art can make various changes and modifications without departing from the spirit and scope of the invention, and therefore all equivalent technical solutions also belong to the scope of the invention.
Those not described in detail in this specification are within the skill of the art.
Claims (10)
1. The continuous basalt fiber surface treating agent is characterized by comprising 100 parts of deionized water, 5-10 parts of a film forming agent, 0.1-0.5 part of a lubricating agent, 0.2-1.0 part of a coupling agent and 0.1-0.5 part of an antistatic agent.
2. The continuous basalt fiber surface treating agent according to claim 1, wherein: the film forming agent is polypropylene grafted maleic anhydride, the grafting rate of the film forming agent is 0.5-2%, 5-10% of emulsifier is contained, and the emulsifier is span-80 or lauryl sodium sulfate.
3. The continuous basalt fiber surface treating agent according to claim 1, wherein: the coupling agent is one or a combination solution of more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
4. The continuous basalt fiber surface treating agent according to claim 1, wherein: the lubricant is one or a mixed solution of more of cationic ammonia or modified silicone oil; the antistatic agent is one or a mixture of more of quaternary ammonium salt and ammonium sulfonate.
5. The method of preparing the continuous basalt fiber surface treating agent according to any one of claims 1 to 4, comprising the steps of: adding 5-10 parts of film forming agent, 0.1-0.5 part of lubricant, 0.2-1.0 part of coupling agent and 0.1-0.5 part of antistatic agent into 100 parts of deionized water by weight, and uniformly stirring at the temperature of 18-25 ℃ to obtain the surface treating agent.
6. A continuous basalt fiber subjected to surface treatment is characterized in that: the surface treatment agent according to any one of claims 1 to 4 is used for surface-treating continuous basalt fibers.
7. The method of preparing a surface-treated continuous basalt fiber according to claim 6, comprising the steps of: and (2) immersing the continuous basalt fiber into a liquid storage tank or a sizing roller in which the treating agent is placed under the action of a traction device, wherein the traction speed is 1-10 m/min, the content of the surface treating agent on the continuous basalt fiber is adjusted through the change of the traction speed, and then drying for 30 min-3 h at the temperature of 80-140 ℃ to obtain the continuous basalt fiber subjected to surface treatment.
8. A continuous basalt fiber reinforced polypropylene composite material is characterized in that: prepared from PP and the surface-treated continuous basalt fiber of claim 6.
9. The method of preparing a continuous basalt fiber reinforced polypropylene composite material according to claim 8, comprising the steps of: and (2) preparing PP and the continuous basalt fiber subjected to surface treatment into a prepreg at 160-200 ℃ by a hot melting method, and further preparing the obtained prepreg into the continuous basalt fiber reinforced polypropylene composite material by a mould pressing process or a vacuum bag process.
10. The method of claim 9, wherein: in the continuous basalt fiber reinforced polypropylene composite material, the mass fraction of the continuous basalt fiber is between 40% and 70%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112724466A (en) * | 2020-12-29 | 2021-04-30 | 江苏绿材谷新材料科技发展有限公司 | Impregnating compound for basalt fiber reinforced polyethylene resin and preparation method thereof |
CN113635571A (en) * | 2021-09-08 | 2021-11-12 | 广西电网有限责任公司电力科学研究院 | Basalt fiber reinforced composite insulating cross arm device and preparation method thereof |
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CN111533467A (en) * | 2020-06-09 | 2020-08-14 | 巨石集团有限公司 | Impregnating compound for glass fiber direct roving and preparation method, product and application thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN112724466A (en) * | 2020-12-29 | 2021-04-30 | 江苏绿材谷新材料科技发展有限公司 | Impregnating compound for basalt fiber reinforced polyethylene resin and preparation method thereof |
CN113635571A (en) * | 2021-09-08 | 2021-11-12 | 广西电网有限责任公司电力科学研究院 | Basalt fiber reinforced composite insulating cross arm device and preparation method thereof |
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