Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
  • D06M13/325—Amines
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
  • D06M13/395—Isocyanates
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/55—Epoxy resins

Definitions

• the present invention relates to a method for producing a modified fiber bundle, and more specifically, a method for producing a modified fiber bundle using fibers used in a fiber-reinforced composite material and a modified fiber bundle obtained by the production method are used. Regarding fiber reinforced composite materials.
• Fiber-reinforced composite materials in which the matrix resin is reinforced with reinforcing fibers such as carbon fiber are lightweight yet have excellent strength, rigidity, dimensional stability, etc., and therefore are used for office equipment, automobiles, aircraft, and vehicles. , IC trays, computer applications such as laptop housings, water stop plates, windmill wings, etc., and their demand is increasing year by year.
• the carbon fiber used for the fiber-reinforced composite material has a different chemical composition and molecular structure from the matrix resin, so that the compatibility with the matrix resin is low, so that the adhesive interface between the carbon fiber and the matrix resin becomes a brittle point and the theoretical strength is high. There is a problem that it cannot be obtained.
• Patent Document 1 proposes improving the compatibility of carbon fibers with a matrix resin by imparting a functional group to the surface of the carbon fibers using a silane coupling agent.
• Patent Document 2 proposes to impart hydrophilicity to carbon fibers by bringing a solution containing trimellitic acid into contact with the carbon fibers.
• Patent Document 3 proposes sizing carbon fibers by using a polymer having a functional group as a sizing agent.
• Patent Document 2 describes the hydrophilicity by trimellitic acid, the majority of trimellitic acid is only retained on the surface of carbon fibers by physical adsorption, and is compatible with the matrix resin. However, there is a problem that the interfacial adhesiveness between the carbon fiber and the trimellitic acid becomes insufficient.
• the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for obtaining a modified fiber bundle having excellent interfacial adhesiveness between a matrix resin and a fiber with high productivity. To do.
• the present inventors have improved the compatibility of the fiber bundle with the matrix resin on the fiber surface and the surface of the sizing agent by contacting the fiber bundle with a modified solution containing a specific nitrogen functional compound and an organic solvent.
• the present invention has been completed by finding that a modified fiber bundle to which a functional group is imparted can be obtained. Further, it has been found that a fiber-reinforced composite material having excellent mechanical properties can be obtained by impregnating the modified fiber bundle thus obtained with a matrix resin. That is, the gist of the present invention is as follows.
• a modification step of contacting a fiber bundle composed of a plurality of fibers with a modification solution containing a nitrogen functional compound and an organic solvent is included.
• the nitrogen functional compound includes at least one functional group of an amino group or an isocyanate group, a vinyl group, an epoxy group, a styryl group, a methacryl group, an acrylic group, a ureido group, a mercapto group, a carboxyl group, an aldehyde group, a ketone group and an amino group.
• a method for producing a modified fiber bundle which is a compound having a molecular weight of 40 or more and 400 or less and having at least one functional group selected from the group consisting of a group, an amide group and an isocyanate group.
• [5] The method for producing a modified fiber bundle according to any one of [1] to [4], wherein the modified solution further contains particles.
• [6] The method for producing a modified fiber bundle according to [5], wherein the particles are inorganic particles.
• the organic solvent contains alcohols having 1 to 10 carbon atoms, ketones having 1 to 6 carbon atoms, sulfoxides having 1 to 10 carbon atoms, esters having 1 to 6 carbon atoms, and 1 to 10 carbon atoms.
• a fiber reinforced composite material with a sheath structure that satisfies [11] The fiber-reinforced composite material of [10], wherein the fiber bundle is a carbon fiber bundle. [12] A surface-modified fiber bundle, which is a surface-modified fiber bundle.
• the nitrogen / carbon ratio and the oxygen / carbon ratio as measured by surface elemental analysis by X-ray photoelectron spectroscopy (ESCA), on the surface of any fiber in the fiber bundle.
• ESA X-ray photoelectron spectroscopy
• N0 / C0> N1 / C1 Satisfied When the oxygen / carbon ratio after etching the fiber surface with Ar gas for 15 seconds is O1 / C1, and the oxygen / carbon ratio after etching with Ar gas for 15 seconds is O2 / C2. O1 / C1> O2 / C2
• a modified fiber bundle having excellent interfacial adhesiveness between a matrix resin and a fiber can be produced with high productivity.
• the fiber-reinforced composite material obtained by impregnating the modified fiber bundle obtained by the production method of the present invention with a matrix resin has few resin-impregnated portions and is excellent in interfacial adhesive strength between fibers and resins, and thus has high mechanical properties. To be equipped.
• the method for producing a modified fiber bundle of the present invention includes a modifying step of bringing a fiber bundle composed of a plurality of fibers into contact with a modifying solution containing a specific nitrogen functional compound and an organic solvent. According to the method for producing a modified fiber bundle of the present invention, a fiber bundle having improved compatibility with a matrix resin can be obtained. The reason is not clear, but it is presumed as follows.
• the amine group or isocyanate group of the nitrogen functional compound becomes a hydroxyl group, a carboxyl group, an aldehyde group, etc. on the fiber surface. It is probable that they reacted and were chemically modified. Further, even when the sizing agent is attached to the fiber surface, the amine group or isocyanate group of the nitrogen functional compound swells the sizing agent on the fiber surface to improve the reactivity, and the amine group or isocyanate group of the nitrogen functional compound.
• the isocyanate group was chemically modified by reacting with the hydroxyl group, carboxyl group, epoxy group and the like on the surface of the sizing agent. In this way, it is considered that the interfacial adhesiveness is also improved by chemically bonding with the sizing agent on the fiber surface and improving the compatibility of the remaining functional groups with the matrix resin.
• the nitrogen functional compound contained in the modified solution has at least one functional group of an amino group or an isocyanate group and at least one other functional group other than the functional group.
• the other functional group is one or more selected from the group consisting of a vinyl group, an epoxy group, a styryl group, a methacryl group, an acrylic group, a ureido group, a mercapto group, an amino group, an amide group, and an isocyanate group. It may be there. It is considered that the amino group or isocyanate group of the nitrogen functional compound chemically bonds with the fiber and the sizing agent, and the other functional groups improve the compatibility with the matrix resin to improve the interfacial adhesiveness.
• the nitrogen functional compound having an amino group or an isocyanate group and a specific other functional group used in the method of the present invention has a molecular weight of 40 or more and 400 or less. If the molecular weight is less than 40, it volatilizes at room temperature (25 ° C.) and is not easy to handle. On the other hand, in the case of a compound having a molecular weight of more than 400, the functional group to react with the matrix resin side is determined from the viewpoint of freedom. There is a high possibility that it will react with the functional groups on the surface of the epoxy resin or carbon resin. For example, Ken Motokura et.
• the preferred molecular weight of the nitrogen functional compound is 50 or more and 300 or less, more preferably 100 or more and 250 or less.
• the reaction with only the surface of the fiber or the sizing agent is suppressed, and the compatibility with the matrix resin tends to be improved.
• a nitrogen functional compound having an aromatic skeleton can be preferably used from the viewpoint of reducing the degree of freedom in the direction of functional groups in the modified solution.
• nitrogen functional compounds examples include urea, allylamine, isocyanate, 2-methylallylamine, 4-vinylaniline, D-alanine, L-alanine, ⁇ -alanine, o-aminobenzoic acid, and m-aminobenzoic acid.
• the concentration of the nitrogen functional compound contained in the modified solution is preferably 0.1 to 20% by mass. Within this concentration range, a fiber bundle having further improved compatibility with the matrix resin can be obtained.
• the concentration of the more preferable nitrogen functional compound is 0.5 to 10% by mass.
• the organic solvent contained in the modifying solution is not particularly limited as long as it is known, but the fiber bundles that are in close contact with each other by electrostatic interaction are dispersed, and the nitrogen functional compound is uniformly reacted on the fiber surface.
• the organic solvent is an alcohol having 1 to 10 carbon atoms such as methanol, ethanol, propanol, isopropanol, n-butyl alcohol and t-butyl alcohol; and 1 to 6 carbon atoms such as acetone, methyl ethyl ketone and methyl isobutyl ketone.
• Ketones sulfoxides having 1 to 10 carbon atoms such as dimethylformamide, dimethylacetamide and dimethylsulfoxide; esters having 1 to 6 carbon atoms such as ethyl acetate and n-butyl acetate; 10 ethers; halogenated hydrocarbons having 1 to 6 carbon atoms such as methylene chloride and chloroform are preferable, and selected from methanol, ethanol, acetone, tetrahydrofuran, chloroform, dimethyl sulfoxide and ethyl acetate capable of softening or dissolving the sizing agent.
• the organic solvent may contain water, or the solvent may be an aqueous solution diluted with water.
• the reforming solution may be an aqueous solution containing an organic solvent component and water.
• the water concentration contained in 100% by mass of the aqueous solution is usually 5 to 95% by mass, preferably 10 to 80% by mass, more preferably 20 to 70% by mass, still more preferably 30 to 60% by mass, most. It is preferably 35 to 55% by mass.
• the water concentration in the organic solvent is not more than the upper limit, it tends to be possible to suppress the complete dissolution of the sizing agent on the fiber surface in the organic solvent.
• the modifying solution contains particles as described below, the particles tend to be able to adhere to the fiber surface.
• the organic solvent component and other components other than water contained in the organic solvent used in the present invention are usually 10% by mass or less, preferably 1% by mass or less, more preferably 0.1% by mass or less, and most preferably. Is only the organic solvent component and water. Inevitable impurities contained in the organic solvent are also included in the organic solvent component (for example, the residual substance in 99.9% absolute ethanol).
• the reforming solution may contain particles.
• the particles By including the particles in the modifying solution, the particles easily adhere to the fiber surface, and the fiber bundle can be opened. As a result, when the fiber-reinforced composite material is obtained, the fiber bundle is easily impregnated with the matrix resin, and the physical properties of the fiber-reinforced composite material tend to be improved.
• the particles include inorganic particles such as silica particles, alumina particles, titanium oxide particles, and carbon particles such as amorphous carbon, and organic particles such as phenol resin particles, polyurethane resin particles, polyamide particles, and polyether ether ketone particles. These particles may be used alone or in combination of two or more. Among these, silica particles and polyetheretherketone particles are preferably used from the viewpoint of affinity with the matrix resin and the sizing agent.
• the average particle size of the particles is preferably 1 to 30 ⁇ m, more preferably 2 to 20 ⁇ m, further preferably 3 to 15 ⁇ m, and particularly preferably 4 to 10 ⁇ m.
• the average particle size of the particles means the median diameter (d50) measured by the laser diffraction method.
• the frequency of particles having a size of 10 ⁇ m or more on a volume basis is preferably 5% or less, more preferably 1% or less.
• the frequency of particles of 1 ⁇ m or less based on the volume is preferably 5% or less, more preferably 1% or less.
• the content of the particles contained in the reforming solution is usually 0.1 part by mass or more, preferably 1 part by mass or more, more preferably 2 parts by mass or more, and further preferably 3 parts by mass with respect to 100 parts by mass of the organic solvent.
• the upper limit is usually 50 parts by mass or less, preferably 30 parts by mass or less, and more preferably 10 parts by mass or less.
• any known reinforcing fiber used in the fiber-reinforced composite material can be used without particular limitation, but carbon fiber can be particularly preferably used.
• the carbon fiber include PAN-based carbon fiber and PITCH-based carbon fiber, and PAN-based carbon fiber is preferably used.
• the average diameter of the fibers is preferably 4 ⁇ m or more, more preferably 6 ⁇ m or more.
• the average diameter of the fibers is preferably 30 ⁇ m or less, more preferably 20 ⁇ m or less.
• the average diameter is an arithmetic mean value of the fiber diameters of 100 randomly selected fibers.
• the fiber diameter means the diameter of this cross section (substantially circular) in the cross section along the direction orthogonal to the length direction of the fiber.
• Each fiber is generally a single fiber (filament), and a plurality of fibers gather to form a fiber bundle (toe).
• the number of fibers constituting each fiber bundle (the number of filaments contained in one strand) is usually 1000 or more, preferably 3000 or more, more preferably 12000 or more, still more preferably 24000 or more.
• the upper limit is not particularly limited, but is usually 100,000 or less, preferably 50,000 or less, more preferably 48,000 or less, and particularly preferably 30,000 or less.
• Fiber bundles can be selected.
• the fiber bundle of the present invention is preferably 48,000 or more and 100,000 or less when unidirectional continuous fibers are used, and 12,000 or more and 48,000 or less when a woven fiber bundle is used.
• the fiber bundle may be used in various forms.
• unidirectional continuous fibers (UniDirection fibers) in which a plurality of fiber bundles are oriented in one direction
• a woven fabric formed by weaving a plurality of fiber bundles
• a knitted fabric formed by knitting a plurality of fiber bundles
• a plurality of fibers It may be used in the form of a non-woven fabric composed of bundles and thermoplastic resin fibers.
• unidirectional continuous fibers and woven fabrics are preferable, and woven fabrics having high mechanical properties in the vertical and horizontal directions are more preferable.
• the woven fabric may be woven in plain weave, twill weave, satin weave or the like, and plain weave or twill weave having isotropic properties is preferable.
• a non-crimp fabric in which the fibers are arranged in a shape having straightness in each fiber orientation direction is preferable.
• the distance between the fibers of the spread fiber bundle is preferably at least a part of 1 ⁇ m or more, preferably 3 ⁇ m or more, and more preferably 5 ⁇ m or more.
• the matrix resin tends to be easily impregnated to the center of the spread fiber bundle by utilizing the voids between the fibers.
• the plurality of fiber bundles are not particularly limited, but are preferably in the form of a sheet.
• Basis weight of the fiber bundle which is a sheet is usually 20 ⁇ 800g / m 2, preferably 100 ⁇ 400g / m 2.
• the basis weight of the fiber bundle is 20 g / m 2 or more, the mechanical strength of the fiber-reinforced composite material formed from the spread fiber bundle of the present invention is improved.
• the basis weight of the fiber bundle is 800 g / m 2 or less, the matrix resin can be uniformly impregnated between the fibers, and the mechanical strength of the fiber-reinforced composite material is improved.
• the basis weight is more preferably 150 to 300 g / m 2 .
• the sizing agent attached to the fiber can be selected according to the matrix resin used for the fiber-reinforced composite material.
• the matrix resin used for the fiber-reinforced composite material.
• epoxy resin, epoxy-modified polyurethane resin, polyester resin, phenol resin, polyamide resin, polyurethane resin, polyimide resin, polyvinyl alcohol resin, polyvinylpyrrolidone resin, polyether sulfone resin and the like are used alone or in combination of two or more. be able to.
• the matrix resin is polypropylene or vinyl chloride resin
• an epoxy resin is preferably used from the viewpoint of interfacial adhesive strength with carbon fibers.
• a sizing agent may be separately added to the fiber to which the sizing agent is not attached, or a commercially available fiber with a sizing agent may be used as it is.
• Examples of commercially available carbon fibers with a sizing agent include TC-33, TC-35, and TC-55 manufactured by Formosa.
• the amount of the sizing agent attached to the fiber bundle of the present invention is not particularly limited, but the sizing agent is usually 0.01 to 10.0% by mass, preferably 0.1 to 7.0% by mass, more preferably 0.1 to 7.0% by mass in the fiber bundle. It is 0.5 to 5.0% by mass, more preferably 1.0 to 3.0% by mass.
• the amount of the sizing agent adhered to the fiber bundle is within the above range, the particles can be adhered to the fiber, and the impregnation property of the matrix resin and the interfacial adhesive strength tend to be improved.
• the method for producing a modified fiber bundle of the present invention includes a step of bringing the fiber bundle into contact with the modified solution.
• Examples of the method of bringing the modified solution into contact with the fiber bundle include a method of immersing the fiber bundle in the modified solution, a method of applying or spraying the modified solution to the fiber bundle, and the like, from the viewpoint of dispersibility of the fiber bundle.
• a method of immersing the fiber bundle in the modifying solution is preferably used.
• the modified solution is usually 1 time or more, preferably 2 times or more, more preferably 8 times or more, based on the total mass of the fibers to be immersed. Is usually 10,000 times or less, preferably 1000 times or less, and more preferably 100 times or less.
• the modified solution is usually 0.01 times or more, preferably 0.1 times or more, more preferably 0.5 times or more, based on the total mass of the fibers to be immersed.
• the upper limit is usually 5 times or less, preferably 3 times or less, and more preferably 1 time or less.
• the temperature of the reforming solution is not particularly limited, but is usually 10 to 50 degrees, preferably 15 to 35 degrees, and more preferably 20 to 25 degrees. The higher the temperature of the reforming solution, the easier it is for the sizing agent to soften, but the cost of maintaining the temperature increases.
• the time for contacting the fiber bundle with the modifying solution can be conveniently adjusted according to the type of sizing agent, but is usually 0.1 seconds or longer, preferably 1 second or longer, more preferably 10 seconds or longer, while The upper limit is usually 60 minutes or less, preferably 30 minutes or less, and more preferably 15 minutes or less.
• the contact time is within the above range, the sizing agent tends to soften and the complete dissolution of the sizing agent in the modified solution tends to be suppressed.
• a sieve or the like may be used to remove particles having a particle size that does not contribute to the opening of the fibers.
• the reaction step may be optionally carried out. It is considered that the reforming reaction proceeds further by heating the fiber bundle after contacting it with the reforming solution.
• the temperature of the reaction step is preferably 200 ° C. or higher from the viewpoint of advancing the reaction.
• the upper limit is usually 400 ° C. or lower, preferably 300 ° C. or lower.
• the heating time when the reaction step is carried out is not particularly limited, but is usually 10 seconds or more, preferably 30 seconds or more, more preferably 1 minute or more, while the upper limit is usually 200 minutes or less, preferably 100 minutes. Below, it is more preferably 30 minutes or less.
• the heating temperature is in the above range, when the reforming solution evaporates, the sizing agent converges on the interface between the particles and the fibers, and the particles tend to adhere to the fiber surface.
• the surface-modified fiber bundle can be obtained as described above, but when the fiber is a carbon fiber, it can be confirmed that the fiber bundle is surface-modified as follows, for example. ..
• the surface element analysis of any fiber surface of the fiber bundle by X-ray photoelectron spectroscopy (ESCA) is performed to calculate the nitrogen / carbon ratio and the oxygen / carbon ratio.
• ESA X-ray photoelectron spectroscopy
• the oxygen / carbon ratio after etching the fiber surface with Ar gas for 15 seconds is O1 / C1
• the oxygen / carbon ratio after etching with Ar gas for 15 seconds is O2 / C2.
• the method for producing a fiber-reinforced composite material of the present invention includes an impregnation step of impregnating the modified fiber bundle obtained as described above with a matrix resin.
• the matrix resin may be either a thermosetting resin or a thermoplastic resin, but from the viewpoint of having a problem of impregnation property and being able to impart an excellent flexural modulus and bending strength to the fiber-reinforced composite material.
• Thermoplastic resin is preferred.
• thermoplastic resin examples include polyolefin resins, acrylic resins, polyamide resins, polycarbonate resins, vinyl chloride resins, aromatic polyetherketones, polyarylene sulfides, and the like, which have a viscosity that affects when impregnated between fibers.
• a polyolefin resin having a good balance of mechanical properties, a vinyl chloride resin having a high viscosity but excellent chemical resistance, and an aromatic polyetherketone having excellent heat resistance are preferable.
• Polyolefin-based resins and vinyl chloride resins are preferably used from the viewpoint of mechanical properties and chemical resistance of the obtained fiber-reinforced composite material.
• polyolefin resin examples include polyethylene resin and polypropylene resin.
• the polyethylene-based resin is not particularly limited, and for example, low-density polyethylene-based resin, medium-density polyethylene-based resin, high-density polyethylene-based resin, linear low-density polyethylene-based resin, linear medium-density polyethylene-based resin, direct Examples include a chain high-density polyethylene resin.
• the polypropylene-based resin is not particularly limited, and examples thereof include a propylene homopolymer and a copolymer of propylene and another olefin.
• the copolymer of propylene and other olefins may be either a block copolymer or a random copolymer.
• propylene and a part of other olefins may be acid-modified with an anhydride or the like.
• Examples of the olefin copolymerized with propylene include ⁇ such as ethylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-octene, 1-nonene, and 1-decene. -Examples include olefins.
• aromatic polyetherketone examples include polyetheretherketone and polyetherketoneketone, and polyetheretherketone is preferably used from the viewpoint of heat resistance and mechanical properties.
• polyphenylene sulfide is preferably used.
• thermosetting resin examples include epoxy resin, unsaturated polyester resin, phenol resin, melamine resin, polyurethane resin and the like, and unsaturated polyester resin and epoxy resin are preferable.
• the content of the spread fiber bundle is preferably 10 to 70% by mass, more preferably 20 to 60% by mass, still more preferably 30 to 50% by mass.
• the content of the matrix resin is preferably 30 to 90% by mass, preferably 40 to 80% by mass, and even more preferably 30 to 60% by mass.
• the method of impregnating the spread fiber bundle with the matrix resin is not particularly limited.
• a method in which a molten resin is extruded into a film using a sheet die or the like, laminated on a fiber-spread fiber bundle, and then compressed while heating to impregnate the matrix resin in the fiber-spread fiber bundle film impregnation method.
• Extrusion molding method that pulls out matrix resin and fibers from the die at once
• Extrusion impregnation method that performs kneading and impregnation at the same time by passing a bundle of spread fibers through the extruder when kneading the resin using an extruder.
• the film impregnation method is preferably used from the viewpoint of productivity.
• the fiber-reinforced composite material of the present invention has the following features. That is, it is a fiber-reinforced composite material containing a surface-modified fiber bundle and a matrix resin.
• the radius of any one fiber is r ( ⁇ m), and at a wavelength R ( ⁇ m) measured by an infrared spectroscope at a distance R ( ⁇ m) from the center of the fiber, at a wavelength of 1724 nm.
• Woven fabric 1 Made by Taiwan Plastics Co., Ltd.
• Product name "EC3C” PAN-based carbon fiber bundle, sizing material: epoxy-based resin, number of filaments: 3000, grain amount: 200 g / m 2 , thickness: 0.19 mm, plain weave
• Woven fabric 2 Made by Toray Industries, Inc.
• Product name "T300B-3K-50B” (3K woven fabric) UD1 Made by Toray Industries, Inc.
• [Resin film] PP1 100 parts by weight of the product name "J108M” (homopolypropylene resin) manufactured by Prime Polymer Co., Ltd. and 10 parts by weight of the product name "Umex 1010" (acid-modified polypropylene) manufactured by Sanyo Kasei Kogyo Co., Ltd.
• PP film PEEK1 manufactured by Solvay after melt-kneading
• PEEK film PPS1 manufactured by Toray Co., Ltd., in which the trade name "Bestakeep KT880-NT” (polyetheretherketone resin) was formed by an extruder.
• Example 1 60 parts by mass of ethanol, 39 parts by mass of distilled water, and 1 part by mass of Compound 1 were mixed to prepare a modified solution having a concentration of nitrogen functional compound of 1% by mass. Subsequently, a modified solution 0.75 times the weight of the carbon fiber bundle of the woven fabric 1 was applied. Then, the obtained carbon fiber bundle was heated at 290 ° C. for 2 minutes and dried.
• the reinforcing fiber bundle is impregnated with the polypropylene resin by compressing the obtained fiber bundle at a pressure of 2 MPa for 3 minutes while heating at 200 ° C.
• a carbon fiber reinforced composite material (prepreg) having a thickness of 250 ⁇ m and a carbon fiber content (volume%) of 50% in the fiber reinforced composite was obtained.
• Example 2 The modification treatment was carried out in the same manner as in Example 1 except that a modification solution having a concentration of 5% by mass of the nitrogen functional compound prepared by mixing 60 parts by mass of ethanol, 35 parts by mass of distilled water and 5 parts by mass of compound 1 was used. And impregnation with a matrix resin was carried out to obtain a carbon fiber reinforced composite material. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 3 Modification treatment using a modification solution having a concentration of 1% by mass of a nitrogen functional compound prepared by mixing 60 parts by mass of ethanol, 37 parts by mass of distilled water, 1 part by mass of compound 2 and 2 parts by mass of particles 1.
• a carbon fiber reinforced composite material was obtained in the same manner as in Example 1 except that PP1 was changed to PPS1 and the impregnation temperature was changed to 320 ° C. as the matrix resin.
• the bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 4 A carbon fiber reinforced composite material was obtained in the same manner as in Example 3 except that compound 2 was changed to compound 3. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 5 A carbon fiber reinforced composite material was obtained in the same manner as in Example 3 except that the woven fabric 1 was changed to UD1, the PPS1 was changed to PEEK1 as the matrix resin, and the impregnation temperature was changed to 360 ° C. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 6 A carbon fiber reinforced composite material was obtained in the same manner as in Example 5 except that compound 2 was changed to compound 3. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 7 A carbon fiber reinforced composite material was obtained in the same manner as in Example 5 except that compound 2 was changed to compound 4. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 1 A carbon fiber reinforced composite material was obtained by performing a modification treatment and impregnation with a matrix resin in the same manner as in Example 1 except that a modification solution prepared by mixing 60 parts by mass of ethanol and 40 parts by mass of distilled water was used. It was. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 2 The modification treatment and impregnation with the matrix resin were carried out in the same manner as in Example 3 except that a modification solution prepared by mixing 60 parts by mass of ethanol, 38 parts by mass of distilled water and 2 parts by mass of particles 1 was used, and carbon was used. A fiber reinforced composite material was obtained. The bending strength of the obtained carbon fiber reinforced composite material was evaluated in the same manner as described above. The results are shown in Table 1.
• Example 3 The modification treatment and impregnation with the matrix resin were carried out in the same manner as in Example 5 except that a modification solution prepared by mixing 60 parts by mass of ethanol, 40 parts by mass of distilled water and 2 parts by mass of particles 1 was used. The bending strength of the carbon fiber reinforced composite material was evaluated.

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• 2020
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