WO2023058694A1 - 赤外線吸収繊維、繊維製品 - Google Patents
赤外線吸収繊維、繊維製品 Download PDFInfo
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- WO2023058694A1 WO2023058694A1 PCT/JP2022/037320 JP2022037320W WO2023058694A1 WO 2023058694 A1 WO2023058694 A1 WO 2023058694A1 JP 2022037320 W JP2022037320 W JP 2022037320W WO 2023058694 A1 WO2023058694 A1 WO 2023058694A1
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- infrared absorbing
- fibers
- absorbing particles
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- fiber
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
Definitions
- the present invention relates to infrared absorbing fibers and textile products.
- the first method is to maintain heat retention by reducing the dissipation of heat generated from the human body.
- a method of physically increasing the air layer in the cold weather clothing by controlling the weaving structure in the cold weather clothing or making the fibers used hollow or porous has been adopted. .
- the heat generated by the human body is radiated back to the human body, or the part of the sunlight received by the cold weather clothing is converted into heat. It is a way to improve Specifically, for example, in cold weather clothing, a method of chemically and physically processing the entire clothing or the fibers constituting the cold weather clothing has been adopted.
- the first method has been to increase the air layer in the clothing, thicken the fabric, make the fabric finer, or darken the color.
- Specific examples include winter clothing such as sweaters, and clothing for winter sports, in which insulation is placed between the outer material and the lining, and the thickness of the air layer in the insulation maintains heat retention. and clothing.
- the air layer is increased by inserting batting, etc., the clothing becomes heavy and bulky, causing problems for sports that require ease of movement.
- the second method described above which actively and effectively utilizes the heat generated internally and the heat from the outside, has begun to be adopted.
- metals such as aluminum and titanium are vapor-deposited on the lining of clothing, etc., and the radiant heat emitted from the body is reflected on the metal vapor-deposited surface, thereby actively dissipating heat.
- the yield deteriorates due to uneven vapor deposition, etc., resulting in an increase in the price of the product itself.
- ceramic particles such as alumina, zirconia, and magnesia are kneaded into the fiber itself, and the far-infrared radiation effect and light of these ceramic particles are converted into heat.
- a method of using the effect of change that is, a method of actively taking in external energy has been proposed.
- Patent Document 1 one or more inorganic fine particles having thermal radiation properties containing at least one metal or metal ion having a thermal conductivity of 0.3 kcal/m 2 ⁇ sec ⁇ °C or more Disclosed is a heat-radiative fiber characterized by containing Silica or barium sulfate are mentioned as inorganic fine particles having thermal radiation properties.
- Patent Document 2 describes a thermoplastic polymer A having a melting point of 110° C. or higher, and a thermoplastic polymer B having a melting point of 15 to 50° C., a cooling crystallization temperature of 40° C. or lower, and a crystallization heat of 10 mJ/mg or higher.
- the conjugate fiber comprises 0.1 to 20% by weight of the fiber weight of ceramic fine particles having far-infrared radiation ability, and the polymer A covers the fiber surface. Thermally insulating composite fibers are disclosed.
- Patent Document 3 discloses an infrared-absorbing processed textile product obtained by dispersing and fixing a binder resin containing an infrared absorber composed of at least one or more predetermined amino compounds in a textile product.
- Patent Document 4 by dyeing with a combination of a dye having a characteristic that the absorption in the near-infrared region is greater than that of a black dye and another dye, the spectral reflection of the fabric in the range of 750 to 1500 nm as the degree of near-infrared absorption
- a near-infrared absorption processing method for a cellulosic fiber structure having a rate of 65% or less is disclosed.
- the applicant of the present invention has proposed fibers containing boride fine particles, tungsten oxide fine particles, composite tungsten oxide fine particles, and textile products obtained by processing the fibers in Patent Documents 5, 6, and 7. are doing.
- infrared absorbing particles such as tungsten oxide fine particles do not have sufficient chemical resistance properties, and infrared absorbing fibers and textile products are exposed to high temperature acid or alkali chemical environments. In some cases, the infrared absorption characteristics were degraded when exposed to
- Patent Document 8 an infrared absorbing fiber with chemical resistance properties
- an object of one aspect of the present invention is to provide an infrared absorbing fiber that has both chemical resistance and excellent infrared absorbing properties.
- fibers and organic-inorganic hybrid infrared absorbing particles In one aspect of the invention, fibers and organic-inorganic hybrid infrared absorbing particles;
- the organic-inorganic hybrid infrared absorbing particles have infrared absorbing particles and a coating resin that covers at least part of the surfaces of the infrared absorbing particles, and the content of the infrared absorbing particles is 15% by mass or more and 55% by mass or less.
- the organic-inorganic hybrid infrared-absorbing particles provide infrared-absorbing fibers disposed in one or more portions selected from the interior and surface of the fibers.
- an infrared absorbing fiber that has both chemical resistance and excellent infrared absorbing properties.
- FIG. 1 is a schematic diagram of the crystal structure of a composite tungsten oxide having a hexagonal crystal structure.
- FIG. 2 is a schematic cross-sectional view of organic-inorganic hybrid infrared absorbing particles.
- FIG. 3 is a schematic cross-sectional view of an infrared absorbing fiber.
- 4 is a transmission electron micrograph of the organic-inorganic hybrid infrared absorbing particles obtained in Example 1.
- the infrared absorbing fiber of this embodiment can contain fibers and organic-inorganic hybrid infrared absorbing particles.
- the organic-inorganic hybrid infrared absorbing particles can have infrared absorbing particles and a coating resin that covers at least part of the surfaces of the infrared absorbing particles.
- the content of the infrared absorbing particles can be 15% by mass or more and 55% by mass or less.
- organic-inorganic hybrid infrared absorbing particles can be arranged in one or more portions selected from the interior and surface of the fiber.
- the infrared absorbing particles such as tungsten oxide fine particles used in infrared absorbing fibers etc. may not have sufficient chemical resistance.
- the inventors of the present invention conducted extensive studies on methods for obtaining infrared absorbing particles that have both chemical resistance and excellent infrared absorbing characteristics.
- Infrared absorbing particles are usually inorganic materials, and it was difficult to arrange organic materials such as resins on at least part of their surfaces. Therefore, organic-inorganic hybrid infrared-absorbing particles and methods for producing them have not been known. In particular, a method for producing organic-inorganic hybrid infrared-absorbing particles with a high content of infrared-absorbing particles as described above has not been known. Therefore, the inventors of the present invention conducted studies and found organic-inorganic hybrid infrared absorbing particles with a high content of infrared absorbing particles, in which an organic material is arranged on at least a part of the surface of the infrared absorbing particles, and a method for producing the same. rice field.
- the infrared absorbing fiber of the present embodiment can contain organic-inorganic hybrid infrared absorbing particles as described above.
- a method for producing the organic-inorganic hybrid infrared absorbing particles may include, for example, the following steps.
- a dispersion preparation process for preparing a dispersion containing infrared absorbing particles, a dispersant, and a dispersion medium.
- a dispersion medium reduction process that evaporates the dispersion medium from the dispersion liquid.
- a raw material mixed liquid preparation process for preparing a raw material mixed liquid by mixing the infrared absorbing particles recovered after the dispersion medium reduction process, the coating resin raw material, the organic solvent, the emulsifier, the water, and the polymerization initiator.
- Dispersion Preparation Step In the dispersion preparation step, a dispersion containing infrared absorbing particles, a dispersant, and a dispersion medium can be prepared.
- Infrared absorbing particles composition, etc.
- various infrared absorbing particles that are required to have improved chemical resistance, such as acid resistance and alkali resistance, can be used as the infrared absorbing particles.
- infrared absorbing particles for example, infrared absorbing particles containing various materials containing free electrons are preferably used, and infrared absorbing particles containing various inorganic materials containing free electrons can be more preferably used.
- infrared-absorbing particles containing one or more selected from oxygen-deficient tungsten oxides and composite tungsten oxides can be particularly preferably used.
- the organic-inorganic hybrid infrared absorbing particles containing the infrared absorbing particles can be made pale and inconspicuous.
- the infrared absorbing particles are, for example, a tungsten oxide represented by the general formula W y O z (W: tungsten, O: oxygen, 2.2 ⁇ z/y ⁇ 2.999), and General formula M x W y O z (element M is H, He, Li, Na, K, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, One or more selected from Hf, Os, Bi, and I, and selected
- materials containing free electrons are known to exhibit a reflection-absorption response to electromagnetic waves around the solar ray region with wavelengths of 200 nm to 2600 nm due to plasma oscillation. Therefore, various materials containing free electrons as described above can be suitably used as the infrared absorbing particles. Infrared absorbing particles, for example, particles smaller than the wavelength of light can reduce geometric scattering in the visible light region (wavelength 380 nm to 780 nm), and can obtain particularly high transparency in the visible light region, which is preferable. .
- transparency is used in the sense of “low scattering and high transmittance of light in the visible light region.”
- tungsten oxide does not have effective free electrons, so it has little absorption/reflection characteristics in the infrared region and is not effective as an infrared absorbing particle.
- WO3 with oxygen deficiency and composite tungsten oxide in which a positive element such as Na is added to WO3 are conductive materials and have free electrons. Analysis of single crystals of materials having these free electrons suggests the response of the free electrons to light in the infrared region.
- Tungsten Oxide Tungsten oxide is represented by the general formula W y O z (where W is tungsten, O is oxygen, and 2.2 ⁇ z/y ⁇ 2.999).
- the composition range of the tungsten and oxygen is such that the composition ratio of oxygen to tungsten (z/y) is preferably less than 3, and 2.2 ⁇ z /y ⁇ 2.999 is more preferable. More preferably, 2.45 ⁇ z/y ⁇ 2.999.
- z/y is 2.2 or more, it is possible to avoid the appearance of an unintended WO2 crystal phase in the tungsten oxide, and to obtain chemical stability as a material. can be made, so it becomes a particularly effective infrared absorbing particle.
- the value of z/y is preferably less than 3, more preferably 2.999 or less, a particularly sufficient amount of free electrons are generated to enhance the absorption and reflection characteristics in the infrared region, resulting in high efficiency. It can be infrared absorbing particles.
- the so-called "Magneli phase” having a composition ratio represented by 2.45 ⁇ z / y ⁇ 2.999 is chemically stable and has excellent light absorption characteristics in the near infrared region, so it can absorb infrared rays. It can be used more preferably as a material. Therefore, it is more preferable that z/y is 2.45 ⁇ z/y ⁇ 2.999 as described above.
- (a2) Composite Tungsten Oxide The composite tungsten oxide is obtained by adding the element M to the WO3 described above.
- x/y which indicates the amount of element M added
- a particularly sufficient amount of free electrons are generated in the composite tungsten oxide, and a high infrared absorption effect can be obtained.
- the amount of the element M added increases, the supply amount of free electrons increases, and the infrared absorption efficiency also increases.
- the value of x/y is 1 or less, it is possible to avoid the generation of an impurity phase in the infrared absorbing particles containing the composite tungsten oxide, which is preferable.
- Element M is H, He, Li, Na, K, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Hf, Os, Bi, It is preferably one or more selected from I.
- the element M is Li, Na, K, Rb, Cs, Fr, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ce, Pr , Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag , Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re It is more preferable to be one or more elements selected from among.
- the element M is selected from alkali metals, alkaline earth metal elements, transition metal elements, 4B group elements, and 5B group elements. More preferably, one or more elements are selected.
- the infrared absorption particles containing the composite tungsten oxide improve the transmission of light in the visible light region and improve the absorption of light in the infrared region.
- FIG. 1 is a schematic plan view of a hexagonal crystal structure.
- FIG. 1 shows a projection view of the crystal structure of a composite tungsten oxide having a hexagonal crystal structure when viewed from the (001) direction, and the unit cell 10 is indicated by a dotted line.
- FIG. 1 six octahedrons 11 formed by 6 units of WO are aggregated to form a hexagonal void 12, and an element 121, which is the element M, is arranged in the void 12 to form one unit. , and a large number of these one units are assembled to form a hexagonal crystal structure.
- the composite tungsten oxide should contain the unit structure described with reference to FIG. Therefore, the composite tungsten oxide may be crystalline or amorphous.
- the hexagonal crystal is likely to be formed.
- elements other than these may be present as long as the above-described element M is present in the hexagonal voids formed by 6 units of WO 2 , and the elements are not limited to the above-described elements.
- the amount of the element M to be added is preferably 0.2 or more and 0.5 or less as the value of x/y in the general formula described above. 0.33 is more preferred. It is considered that the above-described element M is arranged in all the hexagonal voids because the value of x/y is 0.33.
- infrared absorbing particles containing tetragonal and cubic composite tungsten oxides other than hexagonal crystals also have sufficiently effective infrared absorption characteristics.
- the absorption position in the infrared region tends to change, and the absorption position tends to move to the longer wavelength side in the order of cubic ⁇ tetragonal ⁇ hexagonal.
- the absorption of light in the visible region is small in the order of hexagonal crystal, tetragonal crystal, and cubic crystal. Therefore, it is preferable to use a hexagonal composite tungsten oxide for the purpose of transmitting more light in the visible region and shielding more light in the infrared region.
- the tendency of the optical characteristics described here is only a rough tendency, and changes depending on the type of additive element, the amount of addition, and the amount of oxygen, and the present invention is not limited to this.
- Infrared absorbing particles containing tungsten oxide or composite tungsten oxide largely absorb light in the near-infrared region, particularly in the vicinity of a wavelength of 1000 nm.
- the dispersed particle size of the infrared absorbing particles is not particularly limited, and can be selected according to the purpose of use.
- the infrared absorbing particles when used in applications where transparency should be maintained, preferably have a dispersed particle diameter of 800 nm or less. This is because particles with a dispersed particle diameter of 800 nm or less do not completely block light due to scattering, and can maintain visibility in the visible light region and at the same time efficiently maintain transparency. In particular, when the transparency in the visible light region is emphasized, it is preferable to further consider the reduction of scattering due to particles.
- the dispersed particle diameter is preferably 200 nm or less, more preferably 100 nm or less. This is because if the dispersed particle diameter of the particles is small, the scattering of light in the visible light region with a wavelength of 380 nm or more and 780 nm or less due to geometric scattering or Mie scattering is reduced. This is because it is possible to avoid becoming like frosted glass and failing to obtain clear transparency. That is, when the dispersed particle diameter is 200 nm or less, the geometric scattering or Mie scattering is reduced, resulting in a Rayleigh scattering region. This is because, in the Rayleigh scattering region, the scattered light is reduced in proportion to the sixth power of the particle diameter, so that as the dispersed particle diameter is reduced, the scattering is reduced and the transparency is improved.
- the dispersed particle diameter is 100 nm or less, the scattered light is extremely small, which is preferable. From the viewpoint of avoiding light scattering, the smaller the dispersed particle size, the better.
- the lower limit of the dispersed particle size of the infrared absorbing particles is not particularly limited, the dispersed particle size is preferably 1 nm or more because, for example, it can be easily produced industrially.
- the haze value of the infrared absorbing particle dispersion in which the infrared absorbing particles are dispersed in the medium is set to 30% or less with a visible light transmittance of 85% or less. be able to.
- the haze By setting the haze to 30% or less, it is possible to prevent the infrared absorbing particle dispersion from becoming like frosted glass, and to obtain particularly clear transparency.
- the dispersed particle diameter of the infrared absorbing particles can be measured using an ELS-8000 manufactured by Otsuka Electronics Co., Ltd. based on the dynamic light scattering method.
- Crystallite diameter Further, from the viewpoint of exhibiting excellent infrared absorption properties, the crystallite size of the infrared absorbing particles is preferably 1 nm or more and 200 nm or less, more preferably 1 nm or more and 100 nm or less, and 10 nm or more and 70 nm or less. More preferred.
- X-ray diffraction pattern measurement by the powder X-ray diffraction method ( ⁇ -2 ⁇ method) and analysis by the Rietveld method can be used.
- the X-ray diffraction pattern can be measured using, for example, a powder X-ray diffractometer "X'Pert-PRO/MPD" manufactured by PANalytical, Spectris Co., Ltd., or the like.
- Dispersant A dispersant is used for the purpose of hydrophobizing the surface of the infrared absorbing particles.
- the dispersant can be selected according to the dispersion system, which is a combination of the infrared absorbing particles, the dispersion medium, the coating resin raw material, and the like.
- a dispersant having as a functional group one or more selected from an amino group, a hydroxyl group, a carboxyl group, a sulfo group, a phospho group and an epoxy group can be preferably used.
- the infrared absorbing particles are tungsten oxide or composite tungsten oxide
- the dispersant more preferably has an amino group as a functional group.
- the dispersant more preferably has an amino group as a functional group, that is, an amine compound, as described above. Further, the amine compound is more preferably a tertiary amine.
- the dispersant since the dispersant is used for the purpose of hydrophobizing the surface of the infrared absorbing particles, it is preferably a polymeric material.
- the dispersant preferably has one or more selected from, for example, a long-chain alkyl group and a benzene ring. Styrene and tertiary amine 2-(dimethylamino ) polymer dispersants containing ethyl copolymers can be used more preferably.
- the long-chain alkyl group preferably has 8 or more carbon atoms.
- a dispersant that is a polymer material and an amine compound can also be used.
- the amount of the dispersant to be added is not particularly limited and can be arbitrarily selected.
- a suitable amount of the dispersant to be added can be selected according to the type of the dispersant and the infrared absorbing particles, the specific surface area of the infrared absorbing particles, and the like. For example, if the amount of the dispersant to be added is 10 parts by mass or more and 500 parts by mass or less with respect to 100 parts by mass of the infrared absorbing particles, it is preferable because it is easy to prepare a dispersion having a particularly good dispersion state.
- the amount of the dispersant to be added is more preferably 10 parts by mass or more and 100 parts by mass or less, more preferably 15 parts by mass or more and 50 parts by mass or less with respect to 100 parts by mass of the infrared absorbing particles.
- Dispersion medium Any dispersion medium can be used as long as it can disperse the infrared absorbing particles and the dispersant described above to form a dispersion liquid. For example, various organic compounds can be used.
- the dispersion medium for example, one or more selected from aromatic hydrocarbons such as toluene and xylene can be suitably used.
- the dispersion liquid can be prepared by mixing the infrared absorbing particles, the dispersing agent, and the dispersion medium. In order to disperse the particles, it is preferable to pulverize the infrared absorbing particles at the time of mixing.
- the mixing means used when mixing and pulverizing the infrared absorbing particles, the dispersant, and the dispersion medium is not particularly limited, but for example, one or more selected from bead mills, ball mills, sand mills, paint shakers, ultrasonic homogenizers, and the like. can be used.
- a medium stirring mill such as a bead mill, ball mill, sand mill, or paint shaker using medium media such as beads, balls, and Ottawa sand.
- the dispersion medium can be evaporated and dried from the dispersion liquid.
- the dispersion medium reduction step it is preferable to sufficiently evaporate the dispersion medium from the dispersion liquid and recover the infrared absorbing particles.
- a specific means for evaporating the dispersion medium is not particularly limited, but for example, a dryer such as an oven, an evaporator, a vacuum fluidized dryer such as a vacuum grinder, or a spray dryer such as a spray dryer can be used. can.
- the extent to which the dispersion medium is evaporated is not particularly limited, but it is preferable that the content can be sufficiently reduced so that powdery infrared absorbing particles can be obtained, for example, after the dispersion medium reduction step.
- a dispersing agent is arranged around the infrared absorbing particles, and infrared absorbing particles whose surfaces have been hydrophobized can be obtained. For this reason, it is possible to increase the adhesion between the hydrophobicized infrared absorbing particles and the coating resin obtained by polymerizing the coating resin raw material, and the polymerization process described later allows the surface of the infrared absorbing particles to be at least It becomes possible to dispose the coating resin in part.
- (3) Raw material mixture preparation step In the raw material mixture preparation step, the infrared absorbing particles recovered after the dispersion medium reduction step, the coating resin raw material, the organic solvent, the emulsifier, water, and the polymerization initiator are mixed. , a raw material mixture can be prepared.
- the infrared absorbing particles collected after the dispersion medium reduction process may have the dispersant supplied in the dispersion liquid preparation process attached to the surface of the particles and become dispersant-containing infrared absorbing particles. Therefore, when the dispersant is attached to the infrared absorbing particles as described above, the dispersant-containing infrared absorbing particles collected after the dispersion medium reduction step are used as the infrared absorbing particles in the raw material mixture preparation step. become.
- the coating resin raw material is polymerized in the polymerization step described later to become the coating resin arranged on at least a part of the surface of the infrared absorbing particles, and can constitute, for example, a resin capsule. For this reason, various monomers that can form a desired coating resin by polymerization can be selected as the coating resin raw material.
- the coating resin after polymerization is not particularly limited, and may be, for example, one or more resins selected from thermoplastic resins, thermosetting resins, photocurable resins, and the like.
- thermoplastic resins include polyester resins, polycarbonate resins, acrylic resins, polystyrene resins, polyamide resins, vinyl chloride resins, olefin resins, fluorine resins, polyvinyl acetate resins, thermoplastic polyurethane resins, acrylonitrile butadiene styrene resins, polyvinyl Acetal resins, acrylonitrile/styrene copolymer resins, ethylene/vinyl acetate copolymer resins, and the like can be mentioned.
- thermosetting resins examples include phenol resins, epoxy resins, melamine resins, urea resins, unsaturated polyester resins, alkyd resins, thermosetting polyurethane resins, polyimide resins, and silicone resins.
- photocurable resins examples include resins that are cured by irradiation with ultraviolet light, visible light, or infrared light.
- Coating resins include polyester resins, polycarbonate resins, acrylic resins, polystyrene resins, polyamide resins, vinyl chloride resins, olefin resins, fluorine resins, polyvinyl acetate resins, polyurethane resins, acrylonitrile-butadiene-styrene resins, polyvinyl acetal resins, and acrylonitrile.
- styrene copolymer resins ethylene-vinyl acetate copolymer resins, phenol resins, epoxy resins, melamine resins, urea resins, unsaturated polyester resins, alkyd resins, polyimide resins, and silicone resins preferably.
- Both thermoplastic polyurethane resin and thermosetting polyurethane resin can be used as the polyurethane resin.
- a photocurable resin can also be suitably used, and as the photocurable resin, as described above, a resin that is cured by irradiation with any one of ultraviolet light, visible light, and infrared light is preferably used. be able to.
- the coating resin is preferably a resin to which the mini-emulsion polymerization method can be applied, and more preferably contains a polystyrene resin, for example.
- the coating resin is a polystyrene resin
- styrene can be used as the raw material of the coating resin.
- organic solvent has the effect of stabilizing oil droplets, and can also be called a stabilizer, an additive, or the like.
- the organic solvent is also not particularly limited, but it can be anything as long as it is water-insoluble, and is not particularly limited. Among them, those having a low molecular weight are preferable, and examples thereof include long-chain alkyl compounds such as hexadecane, methacrylic acid alkyl esters having a long-chain alkyl moiety such as dodecyl methacrylate and stearyl methacrylate, higher alcohols such as cetyl alcohol, and olive oil. oil, and the like.
- Emulsifier that is, the surfactant, may be cationic, anionic, or nonionic, and is not particularly limited.
- cationic emulsifiers examples include alkylamine salts and quaternary ammonium salts.
- anionic emulsifiers examples include acid salts or ester salts.
- nonionic emulsifiers include various esters, various ethers, various ester ethers, alkanolamides, and the like.
- the emulsifier for example, one or more selected from the above materials can be used.
- a cationic emulsifier that is, a cationic surfactant, from the viewpoint of enabling the infrared absorbing particles to form organic-inorganic hybrid infrared absorbing particles particularly easily.
- cationic emulsifiers selected from dodecyltrimethylammonium chloride (DTAC), cetyltrimethylammonium chloride (CTAC), and the like.
- the emulsifier can be added, for example, to water that is added at the same time, and added as an aqueous solution.
- the critical micelle concentration (CMC) is 10 times or more and 1000 times or less, more preferably 10 times or more and 500 times or less, still more preferably 10 times or more and 300 times or less, particularly preferably 10 times or more and 150 times or less. It is preferable to add as an aqueous solution prepared as follows.
- the content of the infrared-absorbing particles can be 15% by mass or more. That is, by selecting the addition ratio of the emulsifier to the coating resin raw material and the stirring conditions, even when the content ratio of the infrared absorbing particles is 15% by mass or more, resin coating and encapsulation can be performed.
- these conditions change depending on the type of emulsifier, etc., they are not particularly limited, and it is preferable to conduct a preliminary test and select appropriate conditions.
- the polymerization initiator one or more selected from various polymerization initiators such as radical polymerization initiators and ionic polymerization initiators can be used without particular limitation.
- radical polymerization initiators examples include azo compounds, dihalogens, and organic peroxides.
- Redox initiators that combine oxidizing agents and reducing agents, such as hydrogen peroxide and iron(II) salts, persulfates and sodium hydrogen sulfite, can also be mentioned.
- ionic polymerization initiators examples include nucleophiles such as n-butyllithium, electrophiles such as protonic acids, Lewis acids, halogen molecules, and carbocations.
- polymerization initiators examples include 2,2′-azobisisobutyronitrile (AIBN), potassium peroxodisulfate (KPS), 2,2′-azobis(2-methylpropionamidine) dihydrochloride (V-50 ), 2,2′-azobis(2-methyl-N-(2-hydroxyethyl)propionamidine) (VA-086) and the like can be preferably used.
- AIBN 2,2′-azobisisobutyronitrile
- KPS potassium peroxodisulfate
- V-50 2,2′-azobis(2-methylpropionamidine) dihydrochloride
- VA-086 2,2′-azobis(2-methyl-N-(2-hydroxyethyl)propionamidine)
- the polymerization initiator can be added to the organic phase or the aqueous phase depending on its type. can be added to the organic phase and to the aqueous phase when potassium peroxodisulfate (KPS) or 2,2'-azobis(2-methylpropionamidine) dihydrochloride (V-50) is used.
- KPS potassium peroxodisulfate
- V-50 2,2'-azobis(2-methylpropionamidine) dihydrochloride
- the infrared absorbing particles recovered after the dispersion medium reduction step, the coating resin raw material, the organic solvent, the emulsifier, water, and the polymerization initiator are mixed to prepare the raw material mixture.
- the procedure for preparing the raw material mixed solution is not particularly limited, but for example, a mixed solution containing an emulsifier can be prepared in advance as an aqueous phase.
- a mixed solution can be prepared in which the coating resin raw material and the infrared absorbing particles recovered after the dispersion medium reduction step are dispersed in an organic solvent.
- the polymerization initiator can be added to the aqueous phase or the organic phase depending on the type of polymerization initiator used as described above.
- the raw material mixture can be prepared by adding and mixing the organic phase with the aqueous phase.
- the raw material mixed solution preparation step includes a mixing step of mixing the infrared absorbing particles recovered after the dispersion medium reduction step, the coating resin raw material, the organic solvent, the emulsifier, water, and the polymerization initiator, It is preferable to further include a stirring step of stirring the resulting mixture.
- stirring can be performed using, for example, a stirrer.
- the degree of stirring is not particularly limited, but for example, it is preferable to stir so that oil-in-water droplets are formed in which the infrared absorbing particles contained in the coating resin raw material are dispersed in the water phase.
- the stirring step may not be performed, and may be performed together with the stirring step described later.
- the amount of the polymerization initiator to be added is not particularly limited and can be arbitrarily selected.
- the amount of the polymerization initiator to be added can be selected according to the types of the coating resin material and the polymerization initiator, the size of the oil droplets in the mini-emulsion, the ratio of the amount of the coating resin material to the infrared absorbing particles, and the like. For example, if the amount of the polymerization initiator added is 0.01 mol % or more and 1000 mol % or less with respect to the coating resin raw material, it is easy to obtain the organic-inorganic hybrid infrared absorbing particles in which the infrared absorbing particles are sufficiently covered with the coating resin. Therefore, it is preferable.
- the amount of the polymerization initiator to be added is more preferably 0.1 mol % or more and 200 mol % or less, more preferably 0.2 mol % or more and 100 mol % or less, relative to the coating resin raw material.
- the stirring step the raw material mixture obtained in the raw material mixture preparing step can be stirred while being cooled.
- the degree of stirring in the stirring step is not particularly limited and can be selected arbitrarily.
- a mini-emulsion is obtained by adding a substance that is almost insoluble in water, that is, a hydrophobe, to the organic phase and applying a strong shearing force.
- a substance that is almost insoluble in water that is, a hydrophobe
- the hydrophobe include the organic solvent described above in the raw material mixture preparation step.
- the stirring step it is preferable to stir the obtained mini-emulsion so that it has particle size characteristics corresponding to the target organic-inorganic hybrid infrared absorbing particles.
- the stirring step for example, it is preferable to stir the mini-emulsion so that it has one peak in the scattering intensity-based particle size distribution measured by the dynamic light scattering method. That is, in the stirring step, the particle size distribution of the resulting mini-emulsion preferably does not have two or more peaks.
- the particle size distribution of the mini-emulsion obtained in the stirring step is represented by one peak, the organic-inorganic hybrid infrared absorbing particles produced using the mini-emulsion have excellent dispersibility in various media such as dispersion media, An infrared absorbing dispersion, an infrared absorbing dispersion, and an infrared absorbing fiber can be easily formed.
- the infrared absorbing properties of the obtained infrared absorbing dispersion, infrared absorbing dispersion, and infrared absorbing fiber can be particularly enhanced.
- the mini-emulsion obtained in the stirring step preferably has a median diameter D50 of 1 ⁇ m or less and a standard deviation of 500 or less in the particle size distribution based on the scattering intensity measured by the dynamic light scattering method.
- the dispersibility of the organic-inorganic hybrid infrared absorbing particles produced using the miniemulsion is particularly enhanced when used as an infrared absorbing dispersion, an infrared absorbing dispersion, an infrared absorbing fiber, or the like. can be done.
- the standard deviation is set to 500 or less, it is possible to particularly suppress the spread of the particle size distribution of the organic-inorganic hybrid infrared-absorbing particles produced using the miniemulsion.
- the organic-inorganic hybrid infrared-absorbing particles are used to make an infrared-absorbing dispersion, an infrared-absorbing dispersion, an infrared-absorbing fiber, or the like, the infrared-absorbing dispersion, the infrared-absorbing dispersion, or the infrared-absorbing fiber It is easy to disperse uniformly, and it becomes possible to particularly improve the infrared absorption characteristics.
- the above D50 is more preferably 800 nm or less, and even more preferably 500 nm or less.
- the lower limit of D50 is not particularly limited, it is preferably 100 nm or more, more preferably 150 nm or more, from the viewpoint of including a sufficient amount of infrared absorbing particles.
- the standard deviation is more preferably 400 or less, even more preferably 300 or less, and particularly preferably 250 or less.
- the lower limit of the standard deviation is not particularly limited, it is preferably 20 or more, more preferably 50 or more, and even more preferably 100 or more.
- the specific conditions for forming a mini-emulsion with the above particle size characteristics are not particularly limited.
- the conditions of the stirring vessel such as the capacity and the presence or absence of baffle plates, the stirring power, and the stirring to be used, so that an appropriate stirring force can be applied to the raw material mixture.
- Stirring conditions such as the type of means can be selected.
- the stirring process can also be divided and implemented in multiple times, changing stirring conditions.
- the stirring step it is preferable to stir while cooling the raw material mixture as described above. This is because the mini-emulsion can be formed while suppressing the progress of the polymerization reaction by cooling the raw material mixture.
- the degree of cooling the raw material mixed liquid is not particularly limited, but it is preferable to cool the mixed liquid by using a refrigerant of 0° C. or lower, for example, in an ice bath or the like.
- the coating resin raw material can be polymerized after deoxygenation treatment to reduce the amount of oxygen in the raw material mixture.
- the coating resin raw material can be polymerized, and the coating resin can be arranged on at least part of the surface of the infrared absorbing particles.
- the coating resin raw material can be polymerized, and the coating resin can be arranged on at least part of the surface of the infrared absorbing particles.
- the conditions in the polymerization process are not particularly limited, but deoxygenation treatment can be performed to reduce the amount of oxygen in the raw material mixture before starting the polymerization.
- a specific method for the deoxidation treatment is not particularly limited, but examples thereof include a method of irradiating the raw material mixture with ultrasonic waves and a method of blowing an inert gas into the raw material mixture.
- the specific conditions for carrying out the polymerization reaction are not particularly limited because they can be arbitrarily selected according to the coating resin raw material added to the raw material mixture, but for example, the raw material mixture is heated.
- the polymerization reaction can proceed by irradiating with light of a predetermined wavelength.
- an organic material such as a resin is arranged on at least a part of the surface of the infrared absorbing particles, which has been difficult in the past, and the organic-inorganic hybrid Infrared absorbing particles can be obtained. Therefore, even when exposed to high-temperature acid or alkali chemicals, the infrared absorbing particles can be prevented from coming into direct contact with acid or alkali chemicals. can be suppressed.
- organic-inorganic hybrid infrared absorbing particles of the present embodiment it is possible to produce organic-inorganic hybrid infrared absorbing particles with a high infrared absorbing particle content of 15% by mass or more, which has been particularly difficult in the past. Therefore, it is possible to obtain organic-inorganic hybrid infrared-absorbing particles that are excellent not only in chemical resistance properties but also in infrared shielding properties.
- organic-Inorganic Hybrid Infrared Absorbing Particles preferably have infrared absorbing particles and a coating resin that covers at least part of the surface of the infrared absorbing particles. More preferably, the coating resin is a resin capsule, and the infrared absorbing particles are arranged in the resin capsule. That is, it is more preferable that the entire surface of the infrared absorbing particles is covered with the coating resin.
- the organic-inorganic hybrid infrared-absorbing particles can have a content ratio of the infrared-absorbing particles of 15% by mass or more and 55% by mass or less.
- infrared absorbing particles are usually inorganic materials, and it was difficult to place organic materials such as resin on at least part of their surfaces.
- organic materials such as resin
- the inventors of the present invention conducted studies and found that organic-inorganic hybrid infrared absorbing particles having a high content of infrared absorbing particles can be obtained by arranging a resin on at least part of the surface of the infrared absorbing particles.
- the infrared absorbing particles By arranging a coating resin on at least a part of the surface of the infrared absorbing particles, even if the organic-inorganic hybrid infrared absorbing particles are exposed to an environment of chemicals such as high-temperature acids and alkalis, the infrared absorbing particles are It suppresses direct contact with chemical components such as acids and alkalis, and can impart chemical resistance properties. By arranging the infrared absorbing particles in the resin capsule as described above, the chemical resistance can be particularly enhanced.
- the inventors of the present invention conducted further studies, and by using organic-inorganic hybrid infrared absorbing particles with a content ratio of infrared absorbing particles of a predetermined ratio or more, chemical resistance and infrared shielding characteristics are compatible. The present invention has been completed by discovering what the infrared shielding material can do.
- FIG. 2 shows a schematic cross-sectional view of the organic-inorganic hybrid infrared absorbing particles 20 of this embodiment.
- a coating resin 22 is arranged on at least part of the surface of the infrared absorbing particles 21 .
- the organic-inorganic hybrid infrared absorbing particles 20 of the present embodiment preferably have a configuration in which the infrared absorbing particles 21 are arranged in a resin capsule 221 formed of the coating resin 22.
- a plurality of infrared absorbing particles 21 may be arranged in one resin capsule 221, or only one infrared absorbing particle 21 may be arranged. Further, the infrared absorbing particles 21 may be unevenly distributed within the resin capsule 221, but are preferably dispersed.
- At least a portion of the infrared absorbing particles 21 may be covered with the resin capsule 221, and a portion of the infrared absorbing particles 21 may be exposed from the resin capsule 221 to the outer surface.
- the infrared absorbing particles 21 are completely covered with the resin capsule 221 , that is, included in the resin capsule 221 . This is because the infrared absorbing particles 21 are completely covered with the resin capsules 221, so that even when the organic-inorganic hybrid infrared absorbing particles come into contact with various chemical components, the infrared absorbing particles 21 are more reliably in contact with the chemicals. This is because the chemical resistance can be particularly enhanced.
- the organic-inorganic hybrid infrared absorbing particles 20 shown in FIG. 2 are only schematically shown for explanation, and the organic-inorganic hybrid infrared absorbing particles of the present embodiment are not limited to such a form.
- the shape, size, arrangement and distribution of the infrared absorbing particles 21, and the shape and arrangement of the coating resin 22 are not limited to such forms.
- Each member possessed by the organic-inorganic hybrid infrared-absorbing particles The member possessed by the organic-inorganic hybrid infrared-absorbing particles of the present embodiment will be described below.
- (1-1) Coating resin Although the material of the coating resin is not particularly limited, it may contain a resin component, for example.
- the resin component can be selected according to the optical properties required for the organic-inorganic hybrid infrared absorbing particles, and is not particularly limited.
- the coating resin can be one or more resins selected from, for example, thermoplastic resins, thermosetting resins, photo-curing resins, etc., as resin components.
- thermoplastic resins include polyester resins, polycarbonate resins, acrylic resins, polystyrene resins, polyamide resins, vinyl chloride resins, olefin resins, fluorine resins, polyvinyl acetate resins, thermoplastic polyurethane resins, acrylonitrile butadiene styrene resins, polyvinyl Acetal resins, acrylonitrile/styrene copolymer resins, ethylene/vinyl acetate copolymer resins, and the like can be mentioned.
- thermosetting resins examples include phenol resins, epoxy resins, melamine resins, urea resins, unsaturated polyester resins, alkyd resins, thermosetting polyurethane resins, polyimide resins, and silicone resins.
- photocurable resins examples include resins that are cured by irradiation with ultraviolet light, visible light, or infrared light.
- Resins for coating include polyester resins, polycarbonate resins, acrylic resins, polystyrene resins, polyamide resins, vinyl chloride resins, olefin resins, fluororesins, polyvinyl acetate resins, polyurethane resins, acrylonitrile-butadiene-styrene resins, and polyvinyl acetal resins. , acrylonitrile-styrene copolymer resin, ethylene-vinyl acetate copolymer resin, phenol resin, epoxy resin, melamine resin, urea resin, unsaturated polyester resin, alkyd resin, polyimide resin, silicone resin. It is preferable to contain Both thermoplastic polyurethane resin and thermosetting polyurethane resin can be used as the polyurethane resin. Also, the resin component contained in the coating resin can be composed of one or more selected from the above resin group.
- a photocurable resin can also be preferably used, and as the photocurable resin, as described above, a resin that is cured by irradiation with any one of ultraviolet light, visible light, and infrared light can be preferably used.
- the coating resin may contain a photocurable resin as a resin component, and the photocurable resin may contain a resin that is cured by irradiation with any of ultraviolet light, visible light, and infrared light. preferable.
- the resin component contained in the coating resin can also be composed of the above-described photocurable resin.
- the coating resin can be composed only of the resin component, but it can also contain, for example, an emulsifier, a polymerization initiator, and the like added in the manufacturing process.
- (1-2) Infrared Absorbing Particles The infrared absorbing particles have already been explained in the method for producing the organic-inorganic hybrid infrared absorbing particles, so the explanation is omitted. For example, infrared absorbing particles containing various materials containing free electrons can be used. is preferable, and infrared absorbing particles containing various inorganic materials containing free electrons can be more preferably used.
- infrared absorbing particles containing one or more selected from oxygen-deficient tungsten oxides and composite tungsten oxides can be particularly preferably used.
- the infrared absorbing particles are, for example, a tungsten oxide represented by the general formula W y O z (W: tungsten, O: oxygen, 2.2 ⁇ z/y ⁇ 2.999), and General formula M x W y O z (element M is H, He, Li, Na, K, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, S
- the coating resin which is an organic material
- the coating resin is placed on at least part of the surface of the infrared absorbing particles, which has been difficult in the past. Therefore, even if exposed to a chemical environment such as high-temperature acids or alkalis, the infrared absorbing particles can be prevented from coming into direct contact with chemical components such as acids or alkalis, resulting in excellent chemical resistance and reduced infrared absorption characteristics. can be suppressed.
- Infrared absorbing fibers using the organic-inorganic hybrid infrared absorbing particles can also have chemical resistance.
- the content of the infrared absorbing particles in the organic-inorganic hybrid infrared absorbing particles of the present embodiment is preferably 15% by mass or more, more preferably 20% by mass or more.
- the content of the infrared absorbing particles is preferably 55% by mass or less, more preferably 50% by mass or less.
- the organic-inorganic hybrid infrared absorbing particles of the present embodiment have a particle size based on scattering intensity measured by a dynamic light scattering method. It is preferable to have one peak in the distribution. That is, the particle size distribution preferably does not have two or more peaks.
- the particle size distribution of the organic-inorganic hybrid infrared absorbing particles is represented by one peak, it is excellent in dispersibility in various media such as dispersion media. can be easily formed.
- the infrared absorbing properties of the obtained infrared absorbing dispersion, infrared absorbing dispersion, and infrared absorbing fiber can be particularly enhanced.
- the organic-inorganic hybrid infrared absorbing particles of the present embodiment preferably have a median diameter D50 of 1 ⁇ m or less and a standard deviation of 500 or less in the particle size distribution based on the scattering intensity measured by the dynamic light scattering method. .
- D50 By setting D50 to 1 ⁇ m or less, it is possible to particularly improve the dispersibility when making an infrared absorbing dispersion containing organic-inorganic hybrid infrared absorbing particles, an infrared absorbing dispersion, an infrared absorbing fiber, or the like.
- the standard deviation By setting the standard deviation to 500 or less, it is possible to particularly suppress the spread of the particle size distribution of the organic-inorganic hybrid infrared absorbing particles. It is easy to uniformly disperse in an absorbing dispersion, an infrared absorbing dispersion, or an infrared absorbing fiber, and it is possible to particularly improve the infrared shielding properties.
- the above D50 is more preferably 800 nm or less, and even more preferably 500 nm or less.
- the lower limit of D50 is not particularly limited, it is preferably 30 nm or more, more preferably 50 nm or more, and even more preferably 100 nm or more from the viewpoint of encapsulating a sufficient amount of infrared absorbing particles.
- the standard deviation is more preferably 400 or less, even more preferably 300 or less, and particularly preferably 250 or less.
- the lower limit of the standard deviation is not particularly limited, it is preferably 20 or more, more preferably 50 or more, and even more preferably 100 or more.
- the infrared absorbing fiber of this embodiment can contain fibers in addition to the organic-inorganic hybrid infrared absorbing particles described so far.
- the above-described organic-inorganic hybrid infrared absorbing particles are dispersed in an appropriate medium, and the dispersion is contained in one or more portions selected from the inside and the surface of the fiber.
- the fibers possessed by the infrared-absorbing fibers of the present embodiment can include, for example, one or more types selected from synthetic fibers, semi-synthetic fibers, natural fibers, regenerated fibers, and inorganic fibers. Specifically, for example, one or more types selected from a fiber group consisting of synthetic fibers, semi-synthetic fibers, natural fibers, regenerated fibers, and inorganic fibers, or one or more types selected from the above fiber group. Any of one or more types selected from mixed yarns such as blended yarns, combined yarns, and mixed yarns may be used. Considering that the organic-inorganic hybrid infrared-absorbing particles can be contained in the fiber by a simple method and that the heat retention can be maintained, the fiber preferably contains a synthetic fiber, more preferably a synthetic fiber.
- the specific type of the synthetic fiber is not particularly limited.
- Synthetic fibers are selected from, for example, polyurethane fibers, polyamide fibers, acrylic fibers, polyester fibers, polyolefin fibers, polyvinyl alcohol fibers, polyvinylidene chloride fibers, polyvinyl chloride fibers, polyether ester fibers, etc. One or more of the above can be preferably used.
- polyamide fibers include one or more selected from nylon, nylon 6, nylon 66, nylon 11, nylon 610, nylon 612, aromatic nylon, aramid, and the like.
- acrylic fibers include one or more selected from polyacrylonitrile, acrylonitrile-vinyl chloride copolymer, modacrylic, and the like.
- polyester fibers include one or more selected from polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polyethylene naphthalate, and the like.
- the polyolefin fibers include, for example, one or more types selected from polyethylene, polypropylene, polystyrene, and the like.
- polyvinyl alcohol fibers examples include vinylon.
- polyvinylidene chloride fibers examples include vinylidene.
- polyvinyl chloride fibers examples include polyvinyl chloride.
- polyetherester fiber for example, one or more types selected from lexe, success, etc. can be mentioned.
- the infrared absorbing fiber of the present embodiment contains semi-synthetic fiber as fiber
- the semi-synthetic fiber preferably contains one or more selected from, for example, cellulose-based fiber, protein-based fiber, chlorinated rubber, hydrochlorinated rubber, and the like.
- Cellulosic fibers include, for example, one or more selected from acetate, triacetate, acetate oxide, and the like.
- Protein-based fibers include, for example, Promix.
- the natural fibers preferably contain one or more types selected from, for example, plant fibers, animal fibers, mineral fibers, and the like.
- plant fibers include one or more selected from cotton, kapok, flax, hemp, jute, Manila hemp, sisal hemp, New Zealand hemp, Rabu hemp, palm, rush, and straw.
- animal fibers include one or more selected from wool such as wool, goat hair, mohair, cashmere, alpaca, angora, camel, and vicu ⁇ a, silk, down, and feathers.
- the mineral fibers include, for example, one or more types selected from asbestos, asbestos, and the like.
- the infrared absorbing fiber of the present embodiment contains regenerated fibers as fibers
- the regenerated fibers are, for example, one or more selected from cellulose fibers, protein fibers, algin fibers, rubber fibers, chitin fibers, mannan fibers, and the like. It is preferred to include
- Cellulosic fibers include, for example, one or more selected from rayon, viscose rayon, cupra, polynosic, cuprammonium rayon, and the like.
- protein fibers include one or more selected from casein fiber, peanut protein fiber, corn protein fiber, soybean protein fiber, regenerated silk thread, and the like.
- the infrared absorbing fiber of the present embodiment contains inorganic fibers as fibers
- the inorganic fibers preferably contain one or more selected from, for example, metal fibers, carbon fibers, silicate fibers, and the like.
- metal fibers include one or more selected from various metal fibers, gold threads, silver threads, heat-resistant alloy fibers, and the like.
- silicate fibers include one or more selected from glass fibers, slag fibers, rock fibers, and the like.
- the cross-sectional shape of the fiber possessed by the infrared absorbing fiber of the present embodiment is not particularly limited, but may be, for example, one or more selected from circular, triangular, hollow, flat, Y-shaped, star-shaped, core-sheath-shaped, and the like. be done.
- the infrared absorbing fiber of the present embodiment can also contain fibers having different cross-sectional shapes at the same time.
- the organic-inorganic hybrid infrared absorbing particles in one or more portions selected from the interior and surface of the fiber is possible in various ways depending on the cross-sectional shape of the fiber and the like.
- the organic-inorganic hybrid infrared-absorbing particles may be contained in the core portion of the fiber or in the sheath portion.
- the shape of the infrared absorbing fiber of the present embodiment may be filament (long fiber) or staple (short fiber). 4.
- the infrared-absorbing fiber of the present embodiment contains antioxidants, flame retardants, deodorants, insect repellents, antibacterial agents, ultraviolet absorbers, etc., depending on the purpose, within a range that does not impair the performance of the fibers contained. can be contained.
- the infrared absorbing fiber of this embodiment may further contain particles capable of emitting far infrared rays.
- Particles capable of emitting far-infrared radiation can be placed, for example, in one or more portions selected from the interior and surface of the fiber.
- particles capable of emitting far infrared rays include metal oxides such as ZrO 2 , SiO 2 , TiO 2 , Al 2 O 3 , MnO 2 , MgO, Fe 2 O 3 and CuO, ZrC, SiC and TiC.
- At least one selected from carbides such as ZrN, Si 3 N 4 , and nitrides such as AlN can be suitably used.
- the organic-inorganic hybrid infrared-absorbing particles which are an infrared-absorbing material and a near-infrared-absorbing material, possessed by the infrared-absorbing fiber of the present embodiment have the property of absorbing sunlight energy with a wavelength of 0.3 ⁇ m or more and 3 ⁇ m or less, and in particular, the wavelength It selectively absorbs the near-infrared region around 0.9 ⁇ m to 2.2 ⁇ m and converts it into heat or re-radiates it.
- the above-mentioned particles capable of emitting far-infrared rays receive the energy absorbed by the organic-inorganic hybrid infrared-absorbing particles, which are near-infrared absorbing materials, convert the energy into heat energy of middle and far-infrared wavelengths, and radiate it. have the ability.
- ZrO2 particles convert and radiate this energy into thermal energy with a wavelength greater than or equal to 2 ⁇ m and less than or equal to 20 ⁇ m.
- the particles capable of emitting far-infrared rays and the organic-inorganic hybrid infrared-absorbing particles coexist inside or on the surface of the fiber, for example, the solar energy absorbed by the organic-inorganic hybrid infrared-absorbing particles is transferred to the inside of the fiber. ⁇ Efficient consumption on the surface for more effective heat retention.
- FIG. 3 shows a schematic cross-sectional view of a plane passing through the central axis of the infrared absorbing fiber 30 of this embodiment.
- the infrared absorbing fiber 30 of the present embodiment can have organic-inorganic hybrid infrared absorbing particles 32 arranged in one or more portions selected from the interior 31B of the fiber 31 and the surface 31A. That is, in the infrared absorbing fiber 30 of this embodiment, the organic-inorganic hybrid infrared absorbing particles can be arranged on both the inside 31B and the surface 31A of the fiber 31, or on either the inside 31B or the surface 31A of the fiber 31.
- FIG. 3 shows an example in which the organic-inorganic hybrid infrared-absorbing particles 32 are arranged on both the surface 31A and the inside 31B of the fiber 31, but it is not limited to such a form as described above, and it is arranged only on either one.
- FIG. 3 merely shows the infrared absorbing fiber 30 schematically, and the distribution, shape, size, and the like of the organic-inorganic hybrid infrared absorbing particles 32 are not limited to the form.
- the organic-inorganic hybrid infrared absorbing particles have both chemical resistance and excellent infrared absorbing properties. Therefore, the infrared absorbing fiber of the present embodiment containing the organic-inorganic hybrid infrared absorbing particles can also have both chemical resistance and excellent infrared absorbing characteristics. [Method for producing infrared absorbing fiber]
- the method for producing the infrared absorbing fiber of the present embodiment is not particularly limited, and can be produced by arranging organic-inorganic hybrid infrared absorbing particles in one or more portions selected from the surface and inside of the fiber.
- the infrared absorbing fiber of the present embodiment can be manufactured by the following manufacturing methods (a) to (d).
- the organic-inorganic hybrid infrared absorbing particles are uniformly dispersed in advance in a raw material monomer or oligomer solution, and the dispersion is used to synthesize the target raw material polymer, and at the same time, the organic-inorganic hybrid infrared absorbing particles are dispersed.
- Method (a) For example, the case of using polyester fiber as the fiber will be described as an example.
- a dispersion of organic-inorganic hybrid infrared-absorbing particles is added to polyethylene terephthalate resin pellets, which is a thermoplastic resin, mixed uniformly with a blender, and then the solvent is removed.
- the solvent-removed mixture is melt-kneaded with a twin-screw extruder to obtain an organic-inorganic hybrid infrared-absorbing particle-containing masterbatch.
- This organic-inorganic hybrid infrared-absorbing particle-containing masterbatch is melt-mixed near the melting temperature of the resin, and spun according to various known methods, for example.
- a dispersant can be added in order to improve the dispersibility of the organic-inorganic hybrid infrared absorbing particles in the polyethylene terephthalate resin.
- the dispersant is not particularly limited as long as it can disperse the organic-inorganic hybrid infrared absorbing particles in fibers obtained by spinning a polyethylene terephthalate resin or a masterbatch containing the resin.
- the dispersant applied to polyethylene terephthalate resin is not particularly limited, and is preferably, for example, a polymer dispersant such as polyester, polyether, polyacrylic, polyurethane, polyamine, polystyrene.
- main chain selected from system, aliphatic system, or two or more types of unit structures selected from polyester system, polyether system, polyacrylic system, polyurethane system, polyamine system, polystyrene system, and aliphatic system
- a dispersant or the like having a copolymerized main chain is more preferable.
- the dispersant preferably has at least one functional group selected from an amine-containing group, a hydroxyl group, a carboxyl group, a carboxyl group-containing group, a sulfo group, a phosphoric acid group, or an epoxy group.
- polyacrylic resins having amine-containing groups as functional groups are preferred.
- a dispersant having any of the functional groups described above can adsorb to the surface of the organic-inorganic hybrid infrared-absorbing particles and more reliably prevent aggregation of the organic-inorganic hybrid infrared-absorbing particles. Therefore, the organic-inorganic hybrid infrared absorbing particles can be dispersed more uniformly, so that they can be preferably used.
- Such dispersants include Solsperse (registered trademark) (hereinafter the same) 9000, 12000, 17000, 20000, 21000, 24000, 26000, 27000, 28000, 32000, 35100, 54000, and Solsix 250 manufactured by Nippon Lubrizol Co., Ltd.
- Ajisper registered trademark (hereinafter the same) PB821, Ajisper L-Mex, Ajisper 81PB822, Ajisper 8P824 12 ⁇ DisperBYK( ⁇ )( ⁇ )101 ⁇ DisperBYK106 ⁇ DisperBYK108 ⁇ DisperBYK116 ⁇ DisperBYK130 ⁇ DisperBYK140 ⁇ DisperBYK142 ⁇ DisperBYK145 ⁇ DisperBYK161 ⁇ DisperBYK162 ⁇ DisperBYK163 ⁇ DisperBYK164 ⁇ DisperBYK166 ⁇ DisperBYK167 ⁇ DisperBYK168DisperBYK171 ⁇ DisperBYK180 ⁇ DisperBYK182 ⁇ DisperBYK2000 ⁇ DisperBYK2001 ⁇ DisperBYK2009 ⁇ DisperBYK2013 ⁇ DisperBYK2022 ⁇ DisperBYK2025 ⁇ DisperBYK2050 ⁇ DisperBYK2155 ⁇ DisperBYK2164 ⁇ B
- a polymer diol containing organic-inorganic hybrid infrared absorbing particles and an organic diisocyanate are reacted in a twin-screw extruder to synthesize an isocyanate group-terminated prepolymer, which is then reacted with a chain extender to obtain a polyurethane solution (raw polymer ).
- the polyurethane solution is spun according to various known methods.
- Method (d) For example, a case where organic-inorganic hybrid infrared absorbing particles are adhered to the surface of natural fibers will be described as an example.
- a treatment liquid is prepared by mixing organic-inorganic hybrid infrared absorbing particles, one or more binder resins selected from acrylic, epoxy, urethane, and polyester, and a solvent such as water.
- the natural fibers are immersed in the prepared treatment liquid, or the natural fibers are impregnated with the prepared treatment liquid by padding, printing, spraying, or the like, and then dried.
- the organic-inorganic hybrid infrared absorbing particles can be attached to the natural fiber.
- the method (d) can be applied to synthetic fibers, semi-synthetic fibers, regenerated fibers, inorganic fibers, or blended, combined, mixed fibers, etc., in addition to the natural fibers described above.
- the dispersion method for dispersing the organic-inorganic hybrid infrared absorbing particles in a dispersion medium (solvent) is not particularly limited, and the organic-inorganic hybrid infrared absorbing particles are liquid, that is, dispersed. Any method may be used as long as it can be uniformly dispersed in the medium. For example, methods such as medium stirring mill, ball mill, sand mill, and ultrasonic dispersion can be suitably applied.
- the dispersion medium for the organic-inorganic hybrid infrared absorbing particles is not particularly limited, and can be selected according to the fibers to be mixed.
- One or more selected from organic solvents and water can be used.
- the dispersion liquid of the organic-inorganic hybrid infrared absorbing particles may be directly mixed with the fiber or the polymer that is the raw material. do not have. If necessary, an acid or an alkali may be added to the dispersion of the organic-inorganic hybrid infrared absorbing particles to adjust the pH. A surfactant, coupling agent, or the like can also be added.
- the content of the organic-inorganic hybrid infrared-absorbing particles contained in the infrared-absorbing fiber of the present embodiment is not particularly limited.
- the content of the organic-inorganic hybrid infrared-absorbing particles in the infrared-absorbing fiber of the present embodiment is preferably 0.001% by mass or more and 80% by mass or less.
- the content of the organic-inorganic hybrid infrared absorbing particles in the infrared absorbing fiber is 0.005% by mass or more and 50% by mass. The following are more preferable.
- the content of the organic-inorganic hybrid infrared-absorbing particles in the infrared-absorbing fiber is 0.001% by mass or more, a sufficient infrared-absorbing effect can be obtained, for example, even if the fabric using the infrared-absorbing fiber is thin.
- the content of the organic-inorganic hybrid infrared-absorbing particles in the infrared-absorbing fiber is 80% by mass or less, it is preferable, particularly because it is possible to avoid a decrease in spinnability due to clogging of the filter or yarn breakage in the spinning process. It is more preferable if it is 50% by mass or less. Moreover, since the amount of the organic-inorganic hybrid infrared absorbing particles to be added can be small, the physical properties of the fiber are hardly impaired, which is preferable.
- the infrared absorbing fiber according to the present embodiment by arranging infrared absorbing particles inside or on the surface of the fiber, infrared rays from sunlight etc. are efficiently absorbed, and heat retention is excellent. We can provide the best fiber.
- the infrared absorbing fiber according to the present embodiment has high chemical resistance, the infrared absorbing characteristics do not deteriorate even when exposed to a chemical environment such as high-temperature acid or alkali.
- the infrared-absorbing fiber according to the present embodiment can be used in various applications such as winter clothing, sports clothing, stockings, curtains, and other textile products that require heat retention, and other industrial textile products. .
- the textile product of the present embodiment is formed by processing the infrared absorbing fiber described above, and can contain the infrared absorbing fiber described above.
- the textile product of this embodiment can also consist of infrared rays absorption fiber as stated above.
- the textile product of the present embodiment containing the infrared absorbing fiber described above has excellent properties such as a visible light absorptivity of 20% or less and a solar absorptivity of 57% or more.
- a visible light absorptivity of 20% or less and a solar absorptivity of 57% or more indicates that the textile product is light in color and has a better infrared absorption effect.
- the textile product of the present embodiment which contains the infrared absorbing fiber of the present embodiment, has excellent chemical resistance properties. maintains 57% or more of solar radiation absorptivity. That is, the textile product of this embodiment can have chemical resistance properties.
- optical properties of the fiber products obtained in Examples and Comparative Examples were measured using a spectrophotometer U-4100 (manufactured by Hitachi Ltd.). Visible light transmittance, visible light reflectance, solar transmittance, and solar reflectance were measured according to JIS R 3106 (2019).
- the crystallite size of the infrared absorbing particles For the measurement of the crystallite size of the infrared absorbing particles, dry powder of the infrared absorbing particles obtained by removing the solvent from the dispersion liquid of the infrared absorbing particles was used. Then, the X-ray diffraction pattern of the infrared absorbing particles was measured by a powder X-ray diffraction method ( ⁇ -2 ⁇ method) using a powder X-ray diffractometer (X'Pert-PRO/MPD manufactured by PANalytical, Spectris Co., Ltd.). The crystal structure contained in the infrared absorbing particles was identified from the obtained X-ray diffraction pattern, and the crystallite diameter was calculated using the Rietveld method.
- the mini-emulsion obtained in the stirring step and the organic-inorganic hybrid infrared absorbing particles obtained after the polymerization step were measured using a particle size measuring device (ELSZ-2000 manufactured by Otsuka Electronics Co., Ltd.) based on the dynamic light scattering method. Particle size distribution based on scattering intensity was measured, and D50 and standard deviation were calculated.
- Infrared absorbing fibers and textile products were produced and evaluated according to the following procedures. 1. Production of Organic-Inorganic Hybrid Infrared Absorbing Particles Organic-inorganic hybrid infrared absorbing particles used for infrared absorbing fibers were produced according to the following steps. (Dispersion preparation step) In the dispersion preparation step, a dispersion containing infrared absorbing particles, a dispersant, and a dispersion medium was prepared.
- hexagonal cesium tungsten bronze (Cs 0.33 WO z , 2.0 ⁇ z ⁇ 4.0) (YM-01 manufactured by Sumitomo Metal Mining Co., Ltd.) was prepared.
- a polymer dispersant which is a copolymer of styrene and 2-(dimethylamino)ethyl methacrylate, was prepared as the dispersant.
- toluene was prepared as a dispersion medium.
- the crystallite diameter of the recovered infrared absorbing particles that is, the Cs 0.33 WO z particles was measured to be 16 nm.
- the crystallite size was measured and calculated by the method described above.
- (Raw material mixture preparation step) 13.2 g of infrared absorbing particles obtained in the dispersion medium reduction step, 10 g of styrene as a coating resin raw material, 0.5 g of 2,2'-azobisisobutyronitrile as a polymerization initiator, and an organic solvent. 0.7 g of some hexadecane to form an organic phase.
- a raw material mixture was prepared by adding the organic phase to the aqueous phase.
- the raw material mixture prepared in the raw material mixture preparation step is stirred in an ice bath until the particle size distribution based on the scattering intensity measured by the dynamic light scattering method reaches one peak. did At this time, D50 was 188 nm and standard deviation was 119 in the particle size distribution.
- Polymerization process After the stirring step, nitrogen bubbling was performed for 15 minutes on the raw material mixture in an ice bath to deoxygenate it.
- the obtained dispersion containing the organic-inorganic hybrid infrared absorbing particles was diluted, transferred to a microgrid for TEM observation, and the transfer was observed by TEM.
- a TEM image is shown in FIG. From the TEM image, the particles containing composite tungsten oxide that appear black, which are infrared absorbing particles 401, are encapsulated in a polystyrene resin coating that appears gray, which is coating resin 402, to form organic-inorganic hybrid infrared absorbing particles 40. confirmed that there is Note that the microgrid 41 in the TEM image of FIG. 4 does not constitute organic-inorganic hybrid infrared absorbing particles.
- the content of infrared absorbing particles in the organic-inorganic hybrid infrared absorbing particles obtained in Example 1 was 45.4% by mass.
- TGA thermogravimetric measurement
- the resin component is removed by raising the temperature until the weight decrease stops.
- the mass of the infrared absorbing particles in the obtained organic-inorganic hybrid infrared absorbing particles was measured.
- the content ratio of the measured infrared absorbing particles in the organic-inorganic hybrid infrared absorbing particles subjected to the evaluation was calculated.
- Other examples and comparative examples below are calculated in the same manner.
- the obtained organic-inorganic hybrid infrared absorbing particles have one peak in the particle size distribution based on the scattering intensity measured by the dynamic light scattering method, and the D50 calculated from the particle size distribution is 188 nm with a standard deviation of was 119.
- Production of Infrared Absorbing Fiber A dispersion containing the obtained organic-inorganic hybrid infrared absorbing particles was mixed with a water-soluble acrylic binder resin to prepare a treatment liquid. Next, by impregnating the polyester fiber with the prepared treatment liquid and drying it, the infrared absorbing fiber according to Example 1 to which the organic-inorganic hybrid infrared absorbing particles adhere was produced. 3.
- the calculated visible light absorptivity and solar absorptance were 20% and 60%, respectively. Further, when the color tone of the knit product was visually confirmed, it was found to be pale. 5. Evaluation of Alkali Resistance Characteristics
- the textile product according to Example 1 was immersed in a 0.01 mol/L sodium hydroxide aqueous solution maintained at 80° C. for 30 minutes to conduct an alkalinity test. After that, the optical properties were measured again.
- the visible light absorption rate and solar radiation absorption rate after the alkalinity test were 20% and 60%, respectively.
- the difference in visible light absorptance and solar absorptance was 0%.
- the evaluation results are shown in Table 1.
- Example 2 In the raw material mixed solution preparation step, 4.0 g of the infrared absorbing particles obtained in the dispersion medium reduction step of Example 1, 16 g of styrene as a coating resin raw material, and 2,2′-azobisiso as a polymerization initiator 0.8 g of butyronitrile and 1.0 g of hexadecane, an organic solvent, were mixed to form an organic phase.
- Example 2 Separately from the organic phase, 0.5 g of cetyltrimethylammonium chloride, which is an emulsifier, and 80 g of water were mixed to form an aqueous phase.
- An infrared absorbing fiber and a textile product according to Example 2 were obtained in the same manner as in Example 1 except for the above points.
- the content of the infrared absorbing particles in the organic-inorganic hybrid infrared absorbing particles obtained in Example 2 was 16.0% by mass.
- the raw material mixture is stirred in an ice bath until the particle size distribution based on the scattering intensity measured by the dynamic light scattering method reaches one peak.
- the D50 and standard deviation at the time were the same as in Example 1. Further, the obtained organic-inorganic hybrid infrared absorbing particles had one peak in the particle size distribution based on the scattering intensity measured by the dynamic light scattering method, and the D50 and the standard deviation were also the same as in Example 1.
- hexagonal cesium tungsten bronze (Cs 0.33 WO z , 2.0 ⁇ z ⁇ 4.0) (YM-01 manufactured by Sumitomo Metal Mining Co., Ltd.) was prepared.
- An evaporator was used to remove pure water as a dispersion medium from the dispersion of Cs 0.33 WO 2 particles obtained in the dispersion liquid preparation step, and infrared absorbing particles were recovered.
- the collected infrared absorbing particles become dry powder of Cs 0.33 WO z particles.
- the crystallite diameter of the recovered infrared absorbing particles that is, the Cs 0.33 WO z particles was measured to be 16 nm.
- the crystallite size was measured and calculated by the method described above.
- Example except that the dispersion of Cs 0.33 WO z particles according to Comparative Example 1, which was prepared in the dispersion preparation step, was used instead of the dispersion containing the organic-inorganic hybrid infrared-absorbing particles of Example 1.
- An infrared absorbing fiber and a textile product according to Comparative Example 1 were obtained by performing the same operation as in Example 1. The fiber product thus obtained was evaluated in the same manner as in Example 1. The evaluation results are shown in Table 1.
- the content of the infrared absorbing particles in the organic-inorganic hybrid infrared absorbing particles obtained in Comparative Example 2 was 12.7% by mass.
- the raw material mixture was prepared by adding the organic phase to the aqueous phase, but gelation occurred and organic-inorganic hybrid infrared absorbing particles could not be obtained.
- the infrared-absorbing fiber using the organic-inorganic hybrid infrared-absorbing particles of each example and the textile product containing the infrared-absorbing fiber have excellent alkali resistance, that is, excellent chemical resistance, and also have excellent infrared absorption characteristics. did it. Although only the alkalinity test was performed here, these organic-inorganic hybrid infrared absorbing particles also have acid resistance properties because the coating resin is arranged on at least part of the surface of the infrared absorbing particles.
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Abstract
Description
有機無機ハイブリッド赤外線吸収粒子と、を含み、
前記有機無機ハイブリッド赤外線吸収粒子が、赤外線吸収粒子と、前記赤外線吸収粒子の表面の少なくとも一部を覆う被覆用樹脂とを有し、前記赤外線吸収粒子の含有割合が15質量%以上55質量%以下であり、
前記有機無機ハイブリッド赤外線吸収粒子は、前記繊維の内部、および表面から選択された1以上の部分に配置されている赤外線吸収繊維を提供する。
[赤外線吸収繊維]
本実施形態では、赤外線吸収繊維の一構成例について説明する。
1.有機無機ハイブリッド赤外線吸収粒子の製造方法
本実施形態の赤外線吸収繊維は、既述の様に有機無機ハイブリッド赤外線吸収粒子を含有することができる。そして、係る有機無機ハイブリッド赤外線吸収粒子の製造方法は、例えば以下の工程を有することができる。
(1)分散液調製工程
分散液調製工程では、赤外線吸収粒子と、分散剤と、分散媒とを含む分散液を調製することができる。
(a)赤外線吸収粒子
(組成等について)
分散液調製工程においては、赤外線吸収粒子として、耐薬品特性、例えば耐酸性や耐アルカリ性を高めることが求められる各種赤外線吸収粒子を用いることができる。赤外線吸収粒子としては、例えば自由電子を含有する各種材料を含む赤外線吸収粒子を用いることが好ましく、自由電子を含有する各種無機材料を含む赤外線吸収粒子をより好ましく用いることができる。
(a1)タングステン酸化物
タングステン酸化物は、一般式WyOz(但し、Wはタングステン、Oは酸素、2.2≦z/y≦2.999)で表記される。
(a2)複合タングステン酸化物
複合タングステン酸化物は、上述したWO3へ、元素Mを添加したものである。
(分散粒子径)
赤外線吸収粒子の分散粒子径は特に限定されず、その使用目的等によって、選定することができる。
(結晶子径)
また、優れた赤外線吸収特性を発揮させる観点から、赤外線吸収粒子の結晶子径は1nm以上200nm以下であることが好ましく、1nm以上100nm以下であることがより好ましく、10nm以上70nm以下であることがさらに好ましい。結晶子径の測定には、粉末X線回折法(θ-2θ法)によるX線回折パターンの測定と、リートベルト法による解析を用いることができる。X線回折パターンの測定は、例えばスペクトリス株式会社PANalytical製の粉末X線回折装置「X'Pert-PRO/MPD」などを用いて行うことができる。
(b)分散剤
分散剤は、赤外線吸収粒子の表面を疎水化処理する目的で用いられる。分散剤は、赤外線吸収粒子、分散媒、被覆用樹脂原料等の組み合わせである分散系に合わせて選定可能である。中でも、アミノ基、ヒドロキシル基、カルボキシル基、スルホ基、ホスホ基、エポキシ基から選択された1種類以上を官能基として有する分散剤を好適に用いることができる。赤外線吸収粒子がタングステン酸化物や複合タングステン酸化物である場合は、分散剤は、アミノ基を官能基として有することがより好ましい。
(c)分散媒
分散媒は、既述の赤外線吸収粒子、および分散剤を分散し、分散液とすることができるものであれば良く、例えば各種有機化合物を用いることができる。
(2)分散媒低減工程
分散媒低減工程では、分散液から分散媒を蒸発、乾燥させることができる。
(3)原料混合液調製工程
原料混合液調製工程では、分散媒低減工程後に回収した赤外線吸収粒子と、被覆用樹脂原料と、有機溶媒と、乳化剤と、水と、重合開始剤とを混合し、原料混合液を調製することができる。
(a)被覆用樹脂原料
被覆用樹脂原料は、後述する重合工程で重合し、赤外線吸収粒子の表面の少なくとも一部に配置される被覆用樹脂となり、例えば樹脂カプセルを構成できる。このため、被覆用樹脂原料としては、重合することにより、所望の被覆用樹脂を形成できる各種モノマー等を選択することができる。
(b)有機溶媒
有機溶媒は、油滴を安定化させる効果を有し、安定剤、添加剤等と呼ぶこともできる。
(c)乳化剤
乳化剤、すなわち界面活性剤については、カチオン性のもの、アニオン性のもの、ノニオン性のもの等のいずれでもよく、特に限定されない。
(d)重合開始剤
重合開始剤としては、ラジカル重合開始剤、イオン重合開始剤等の各種重合開始剤から選択された1種類以上を用いることができ、特に限定されない。
(4)攪拌工程
攪拌工程では、原料混合液調製工程で得られた原料混合液を冷却しつつ、攪拌することができる。
(5)重合工程
重合工程では、原料混合液中の酸素量を低減する脱酸素処理を行った後、被覆用樹脂原料の重合反応を行うことができる。
2.有機無機ハイブリッド赤外線吸収粒子
本実施形態の有機無機ハイブリッド赤外線吸収粒子は、赤外線吸収粒子と、赤外線吸収粒子の表面の少なくとも一部を覆う被覆用樹脂とを有することが好ましい。なお、被覆用樹脂は樹脂カプセルとなり、赤外線吸収粒子は該樹脂カプセル中に配置されていることがより好ましい。すなわち、赤外線吸収粒子は、その表面全体が被覆用樹脂により覆われていることがより好ましい。
(1)有機無機ハイブリッド赤外線吸収粒子が有する各部材について
本実施形態の有機無機ハイブリッド赤外線吸収粒子が有する部材について以下に説明する。
(1-1)被覆用樹脂
被覆用樹脂の材料は特に限定されないが、例えば樹脂成分を含有できる。樹脂成分は、有機無機ハイブリッド赤外線吸収粒子に要求される光学特性等に応じて選択でき、特に限定されない。被覆用樹脂は、樹脂成分として、例えば熱可塑性樹脂、熱硬化性樹脂、光硬化樹脂等から選択された1種類以上の樹脂とすることができる。
(1-2)赤外線吸収粒子
赤外線吸収粒子については、有機無機ハイブリッド赤外線吸収粒子の製造方法において既に説明したため、説明を省略するが、例えば自由電子を含有する各種材料を含む赤外線吸収粒子を用いることが好ましく、自由電子を含有する各種無機材料を含む赤外線吸収粒子をより好ましく用いることができる。
(2)赤外線吸収粒子の含有割合について
本発明の発明者の検討によれば、有機無機ハイブリッド赤外線吸収粒子とすることで、耐薬品特性を高められるが、特に高い赤外線遮蔽特性を発揮するためには赤外線吸収粒子の含有割合を高める必要がある。
(3)有機無機ハイブリッド赤外線吸収粒子の粒度分布について
本発明の発明者の検討によれば、本実施形態の有機無機ハイブリッド赤外線吸収粒子は、動的光散乱方式により測定される散乱強度基準の粒度分布において、1つのピークを有することが好ましい。すなわち、上記粒度分布は、2つ以上の複数のピークを有しないことが好ましい。このように有機無機ハイブリッド赤外線吸収粒子の粒度分布が1つのピークにより表される場合、分散媒等の各種媒体への分散性に優れるため、赤外線吸収分散液や、赤外線吸収分散体、赤外線吸収繊維を容易に形成できる。また、得られた赤外線吸収分散液や、赤外線吸収分散体、赤外線吸収繊維の赤外線吸収特性を特に高めることができる。
3.繊維
本実施形態の赤外線吸収繊維が有する繊維は、用途に応じて各種選択可能である。
4.添加剤
本実施形態の赤外線吸収繊維は、含有する繊維の性能を損なわない範囲内で、目的に応じて、酸化防止剤、難燃剤、消臭剤、防虫剤、抗菌剤、紫外線吸収剤等を含有できる。
[赤外線吸収繊維の製造方法]
例えば、繊維としてポリエステル系繊維を用いる場合を例に説明する。
(a)と同様の方法などを活用して、有機無機ハイブリッド赤外線吸収粒子含有マスターバッチを作製し、該マスターバッチと、有機無機ハイブリッド赤外線吸収粒子無添加のポリエチレンテレフタレートよりなるマスターバッチとを、所望の混合比となるように、樹脂の溶融温度付近で溶融混合し公知の方法に従って紡糸する。
例えば、繊維としてウレタン繊維を用いる場合を例に説明する。
例えば、天然繊維の表面に有機無機ハイブリッド赤外線吸収粒子を付着させる場合を例に説明する。
[繊維製品]
本実施形態の繊維製品は、既述の赤外線吸収繊維を加工してなり、既述の赤外線吸収繊維を含むことができる。なお、本実施形態の繊維製品は既述の赤外線吸収繊維からなることもできる。
[実施例1]
以下の手順により赤外線吸収繊維、繊維製品を作製し、評価を行った。
1.有機無機ハイブリッド赤外線吸収粒子の製造
以下の工程に従い、赤外線吸収繊維に用いる有機無機ハイブリッド赤外線吸収粒子の製造を行った。
(分散液調製工程)
分散液調製工程では、赤外線吸収粒子と、分散剤と、分散媒とを含む分散液を調製した。
(分散媒低減工程)
分散液調製工程で得られたCs0.33WOz粒子の分散液からエバポレーターを用いて分散媒のトルエンを除去し、赤外線吸収粒子を回収した。回収した赤外線吸収粒子は、高分子分散剤を含有するCs0.33WOz粒子の乾粉となる。
(原料混合液調製工程)
分散媒低減工程で得られた赤外線吸収粒子13.2gと、被覆用樹脂原料であるスチレン10gと、重合開始剤である2,2'-アゾビスイソブチロニトリル0.5gと、有機溶媒であるヘキサデカン0.7gとを混合し、有機相を形成した。
(攪拌工程)
原料混合液調製工程で調製した原料混合液に対して、氷浴下で、得られるミニエマルションについて、動的光散乱方式により測定される散乱強度基準の粒度分布が、1つのピークとなるまで攪拌を行った。この際、上記粒度分布において、D50が188nm、標準偏差が119であった。
(重合工程)
攪拌工程後、原料混合液に対して、氷浴下で窒素バブリングを15分間行い、脱酸素処理を行った。
2.赤外線吸収繊維の製造
得られた有機無機ハイブリッド赤外線吸収粒子を含む分散液と水溶性のアクリル系のバインダー樹脂とを混合し、処理液を調製した。次に、調製された処理液にポリエステル系繊維を含侵させて乾燥することで、有機無機ハイブリッド赤外線吸収粒子が付着した実施例1に係る赤外線吸収繊維を作製した。
3.繊維製品の製造
得られた赤外線吸収繊維を切断してポリエステルステープルを作製し、これを用いて紡績糸を製造した。そして、この紡績糸を用いて実施例1に係るニット製品を得た。なお、作製されたニット製品試料の日射吸収率は60%前後となるように調整した。以下の他の実施例、比較例においても同様に調整した。
4.繊維製品の評価
実施例1に係る繊維製品の光学特性を、上述の方法により測定した。当該可視光吸収率と日射吸収率は、可視光吸収率(%)=100%-可視光透過率(%)-可視光反射率(%)および日射吸収率(%)=100%-日射透過率(%)-日射反射率(%)から算出した。算出された可視光吸収率と日射吸収率は、それぞれ20%と60%であった。また、ニット製品の色調を目視で確認したところ、淡色であった。
5.耐アルカリ特性の評価
実施例1に係る繊維製品を、80℃に保持した0.01mol/Lの水酸化ナトリウム水溶液に30分間浸漬し、アルカリ性試験を行った。その後、再度光学特性を測定した。
[実施例2]
原料混合液調製工程において、実施例1の分散媒低減工程で得られた赤外線吸収粒子4.0gと、被覆用樹脂原料であるスチレン16gと、重合開始剤である2,2'-アゾビスイソブチロニトリル0.8gと、有機溶媒であるヘキサデカン1.0gとを混合して有機相を形成した。
[比較例1]
分散液調製工程では、赤外線吸収粒子と、分散媒とを含む分散液を調製した。
[比較例2]
原料混合液調製工程において、実施例1の分散媒低減工程で得られた赤外線吸収粒子3.9gと、被覆用樹脂原料であるスチレン20.9gと、重合開始剤である2,2'-アゾビスイソブチロニトリル0.8gと、有機溶媒であるヘキサデカン2.0gとを混合して有機相を形成した。
[比較例3]
原料混合液調製工程において、実施例1の分散媒低減工程で得られた赤外線吸収粒子3.9gと、被覆用樹脂原料であるスチレン0.8gと、重合開始剤である2,2'-アゾビスイソブチロニトリル0.8gと、有機溶媒であるヘキサデカン2.0gとを混合して有機相を形成した。
21、401 赤外線吸収粒子
22、402 被覆用樹脂
221 樹脂カプセル
30 赤外線吸収繊維
31 繊維
31A 表面
31B 内部
Claims (11)
- 繊維と、
有機無機ハイブリッド赤外線吸収粒子と、を含み、
前記有機無機ハイブリッド赤外線吸収粒子が、赤外線吸収粒子と、前記赤外線吸収粒子の表面の少なくとも一部を覆う被覆用樹脂とを有し、前記赤外線吸収粒子の含有割合が15質量%以上55質量%以下であり、
前記有機無機ハイブリッド赤外線吸収粒子は、前記繊維の内部、および表面から選択された1以上の部分に配置されている赤外線吸収繊維。 - 前記被覆用樹脂が、ポリエステル樹脂、ポリカーボネート樹脂、アクリル樹脂、ポリスチレン樹脂、ポリアミド樹脂、塩化ビニル樹脂、オレフィン樹脂、フッ素樹脂、ポリ酢酸ビニル樹脂、ポリウレタン樹脂、アクリロニトリルブタジエンスチレン樹脂、ポリビニルアセタール樹脂、アクリロニトリル・スチレン共重合体樹脂、エチレン・酢酸ビニル共重合体樹脂、フェノール樹脂、エポキシ樹脂、メラミン樹脂、尿素樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリイミド樹脂、シリコーン樹脂から選択された1種類以上を含有する請求項1に記載の赤外線吸収繊維。
- 前記被覆用樹脂が、光硬化樹脂であり、該光硬化樹脂が紫外線、可視光線、赤外線のいずれかの光の照射により硬化する樹脂を含有する請求項1または請求項2に記載の赤外線吸収繊維。
- 前記赤外線吸収粒子が、一般式WyOz(W:タングステン、O:酸素、2.2≦z/y≦2.999)で表されるタングステン酸化物、および一般式MxWyOz(元素MはH、He、Li、Na、K、Rb、Cs、Fr、Be、Mg、Ca、Sr、Ba、Ra、Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Zr、Cr、Mn、Fe、Ru、Co、Rh、Ir、Ni、Pd、Pt、Cu、Ag、Au、Zn、Cd、Al、Ga、In、Tl、Si、Ge、Sn、Pb、Sb、B、F、P、S、Se、Br、Te、Ti、Nb、V、Mo、Ta、Re、Hf、Os、Bi、Iのうちから選択された1種類以上、0.001≦x/y≦1、2.0≦z/y<4.0)で表される複合タングステン酸化物から選択された1種類以上を含有する請求項1から請求項3のいずれか1項に記載の赤外線吸収繊維。
- 前記繊維が合成繊維、半合成繊維、天然繊維、再生繊維、無機繊維から選択された1種類以上を含む請求項1から請求項4のいずれか1項に記載の赤外線吸収繊維。
- 前記合成繊維が、ポリウレタン繊維、ポリアミド系繊維、アクリル系繊維、ポリエステル系繊維、ポリオレフィン系繊維、ポリビニルアルコール系繊維、ポリ塩化ビニリデン系繊維、ポリ塩化ビニル系繊維、ポリエーテルエステル系繊維から選択された1種類以上を含む請求項5に記載の赤外線吸収繊維。
- 前記半合成繊維がセルロース系繊維、タンパク質系繊維、塩化ゴム、塩酸ゴムから選択された1種類以上を含む請求項5または請求項6に記載の赤外線吸収繊維。
- 前記天然繊維が植物繊維、動物繊維、鉱物繊維から選択された1種類以上を含む請求項5から請求項7のいずれか1項に記載の赤外線吸収繊維。
- 前記再生繊維が、セルロース系繊維、タンパク質系繊維、アルギン繊維、ゴム繊維、キチン繊維、マンナン繊維から選択された1種類以上を含む請求項5から請求項8のいずれか1項に記載の赤外線吸収繊維。
- 前記無機繊維が金属繊維、炭素繊維、珪酸塩繊維から選択された1種類以上を含む請求項5から請求項9のいずれか1項に記載の赤外線吸収繊維。
- 請求項1から請求項10のいずれか1項に記載の赤外線吸収繊維を含む繊維製品。
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