WO2013008807A1 - Agent antiviral apte à inactiver un virus, et procédé d'inactivation d'un virus - Google Patents

Agent antiviral apte à inactiver un virus, et procédé d'inactivation d'un virus Download PDF

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Publication number
WO2013008807A1
WO2013008807A1 PCT/JP2012/067559 JP2012067559W WO2013008807A1 WO 2013008807 A1 WO2013008807 A1 WO 2013008807A1 JP 2012067559 W JP2012067559 W JP 2012067559W WO 2013008807 A1 WO2013008807 A1 WO 2013008807A1
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virus
photocatalyst
noble metal
antiviral agent
particles
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PCT/JP2012/067559
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English (en)
Japanese (ja)
Inventor
酒谷　能彰
仁 高見
康平 曽我部
一明 竹原
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住友化学株式会社
国立大学法人東京農工大学
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Publication of WO2013008807A1 publication Critical patent/WO2013008807A1/fr

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00—Disinfection, sterilisation or deodorisation of air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/652—Chromium, molybdenum or tungsten
    • B01J23/6527—Tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
    • B01J23/687—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0215—Coating
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
    • A61L2/08—Radiation
    • A61L2/10—Ultraviolet radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst

Definitions

  • the present invention relates to an antiviral agent for inactivating viruses and a method for inactivating viruses.
  • Non-Patent Document 1 Non-Patent Document 1
  • an antiviral agent in which a photocatalyst of a bowl-shaped crystal particle and a photocatalyst of a spherical crystal particle are bonded through an OH group inactivates avian influenza virus under irradiation of a fluorescent lamp.
  • Patent Document 1 An antiviral agent in which a photocatalyst of a bowl-shaped crystal particle and a photocatalyst of a spherical crystal particle are bonded through an OH group inactivates avian influenza virus under irradiation of a fluorescent lamp.
  • An object of the present invention is to provide an antiviral agent capable of expressing a high antiviral property even under irradiation with visible light and inactivating a virus having high resistance, and a method for inactivating the virus. .
  • the present inventors inactivate even a relatively small virus having no extremely high envelope by supporting a predetermined amount of noble metal on the photocatalyst particles.
  • the present invention has been completed. That is, the present invention (1) An antiviral agent comprising a photocatalyst structure provided on the surface with a photocatalyst layer comprising a photocatalyst particle carrying a noble metal particle and a binder, and the antiviral agent comprising 100 parts by mass of the photocatalyst particle 0.01 to 1 part by mass of noble metal particles are supported, An antiviral agent that inactivates a virus having a size of 15 to 30 nm and having no envelope; (2) The antiviral agent according to (1), wherein the photocatalyst particles are tungsten oxide particles, (3) The antiviral agent according to (1) or (2), wherein the noble metal is at least one kind of noble metal selected from the group consisting of Cu, Pt, Au, Pd,
  • Method (8) The method for inactivating the virus according to any one of (5) to (7), wherein the binder comprises a silicon alkoxide, (9) Ceiling material, tile, glass, wallpaper, wall material, film, floor, fence, tatami, shoji selected from the group consisting of shoji, or automotive instrument panel, car seat, car ceiling material Automotive interior materials selected from the group consisting of automotive glass, or the group consisting of refrigerators, air conditioners, personal computers, printers, scanners, photocopiers, fax machines, telephones, TVs, stereos, washing machines, stoves, dryers, microwave ovens More selected household appliances, furniture selected from the group consisting of desks, chairs, tables, bags, storage shelves, textiles selected from the group consisting of clothes, curtains, railings, trains Any one of (1) to (4) for a base material that can be contacted by an unspecified number of people selected from the group consisting of straps and elevator buttons Use of anti-viral agents described, It is in.
  • inactivating the virus means that when the virus titer (50% tissue culture infectious amount per ml: TCID 50 / ml) is calculated by the Behrens Kerber method, the virus titer is calculated. This means that the logarithmic value (log 10) of ⁇ decreases by 1.5 or more, preferably by 2.5 or more.
  • an antiviral agent capable of expressing a high antiviral property even under visible light irradiation and inactivating a virus having high resistance, and a method of inactivating the virus. Can do.
  • Embodiment 1 illustrates the antiviral agent of this invention, Comprising: This invention is not limited to the following.
  • the antiviral agent according to Embodiment 1 is an antiviral agent comprising a photocatalyst structure having on its surface a photocatalyst layer comprising a photocatalyst particle carrying precious metal particles and a binder.
  • the precious metal particles are supported in an amount of 0.01 to 1 part by mass with respect to 100 parts by mass of the particles, and inactivate viruses having a size of 15 to 30 nm and having no envelope. To do.
  • the photocatalyst particle used in the present invention refers to a particulate photocatalyst.
  • the photocatalyst include a compound of a metal element and oxygen, nitrogen, sulfur, and fluorine.
  • metal elements include Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt, and Cu. , Ag, Au, Zn, Cd, Ga, In, Tl, Ge, Sn, Pd, Bi, La, and Ce.
  • Examples of the compound include one or more oxides, nitrides, sulfides, oxynitrides, oxysulfides, nitrofluorides, oxyfluorides, and oxynitrofluorides of these metal elements.
  • tungsten oxide is preferably used in the present invention because it exhibits high antiviral activity when irradiated with visible light (wavelength of about 400 nm to about 800 nm).
  • the photocatalyst particles usually have an average dispersed particle diameter of 40 nm to 250 nm.
  • the tungsten oxide particles include, for example, (i) a method of adding tungstic acid as a precipitate by adding an acid to an aqueous solution of tungstate, and firing this tungstic acid, (ii) meta It can be obtained by a method of thermally decomposing by heating ammonium tungstate or ammonium paratungstate, or (iii) a method of firing metallic tungsten particles.
  • the photocatalyst particles are usually mixed with a binder in the state of a photocatalyst dispersion dispersed in an appropriate dispersion medium.
  • the photocatalyst dispersion liquid may be prepared by dispersing photocatalyst particles in a dispersion medium.
  • a dispersion treatment with a known apparatus such as a wet medium stirring mill.
  • the aqueous solvent which has water as a main component is used.
  • the dispersion medium may be water alone or a mixed solvent of water and a water-soluble organic solvent.
  • a mixed solvent of water and a water-soluble organic solvent is used, the content of water is preferably 50% by mass or more.
  • the water-soluble organic solvent include water-soluble alcohol solvents such as methanol, ethanol, propanol, and butanol, acetone, methyl ethyl ketone, ethyl cellosolve, butyl cellosolve, ethyl acetate, diethyl ether, and the like.
  • a dispersion medium may be used independently and may use 2 or more types together.
  • the amount of the dispersion medium used is usually 2 to 200 times the mass of the photocatalyst particles. If the amount of the dispersion medium used is less than 2 mass times, the photocatalyst particles are likely to settle, and if it exceeds 200 mass times, it is disadvantageous in terms of volume efficiency.
  • Noble metal particles are supported on the photocatalyst particles of the present invention.
  • the noble metal particles can be supported by a known method such as an impregnation method, a coprecipitation method, or a photo-deposition method using a precursor of a noble metal.
  • the noble metal particles are dispersed in a highly dispersed state in the photocatalyst particles. Since it can carry
  • the precious metal precursor one that can be dissolved in a dispersion medium is used.
  • the noble metal element constituting the precursor usually becomes a noble metal ion having a positive charge and exists in the dispersion medium.
  • this noble metal ion is reduced to a zero-valent noble metal by light irradiation and is supported on the surface of the photocatalyst particles.
  • the noble metal include Cu, Pt, Au, Pd, Ag, Ru, Ir, and Rh.
  • the precursor include hydroxides, nitrates, sulfates, halides, organic acid salts, carbonates, and phosphates of these noble metals.
  • the noble metal is preferably Cu, Pt, Au, or Pd, and among these, Pt is particularly preferable.
  • Cu As a precursor of Cu, for example, copper nitrate (Cu (NO 3 ) 2 ), copper sulfate (CuSO 4 ), copper chloride (CuCl 2 , CuCl), copper bromide (CuBr 2 , CuBr), copper iodide (CuI) , Copper iodate (CuI 2 O 6 ), copper copper chloride (Cu (NH 4 ) 2 Cl 4 ), copper oxychloride (Cu 2 Cl (OH) 3 ), copper acetate (CH 3 COOCu, (CH 3 COO) 2 Cu), copper formate ((HCOO) 2 Cu), copper carbonate (CuCO 3 ), copper oxalate (CuC 2 O 4 ), copper citrate (Cu 2 C 6 H 4 O 7 ), copper phosphate (CuPO 4) ).
  • Pt precursors include platinum chloride (PtCl 2 , PtCl 4 ), platinum bromide (PtBr 2 , PtBr 4 ), platinum iodide (PtI 2 , PtI 4 ), potassium tetrachloroplatinate (K 2 PtCl 4 ).
  • Au precursor examples include gold chloride (AuCl), gold bromide (AuBr), gold iodide (AuI), gold hydroxide (Au (OH) 2 ), tetrachloroauric acid (HAuCl 4 ), tetra
  • Au precursor examples include gold chloride (AuCl), gold bromide (AuBr), gold iodide (AuI), gold hydroxide (Au (OH) 2 ), tetrachloroauric acid (HAuCl 4 ), tetra
  • Au precursor examples include gold chloride (AuCl), gold bromide (AuBr), gold iodide (AuI), gold hydroxide (Au (OH) 2 ), tetrachloroauric acid (HAuCl 4 ), tetra
  • K chloroaurate K tetrabromoaurate (KAuBr 4 ).
  • Examples of the precursor of Pd include palladium acetate ((CH 3 COO) 2 Pd), palladium chloride (PdCl 2 ), palladium bromide (PdBr 2 ), palladium iodide (PdI 2 ), palladium hydroxide (Pd ( OH) 2 ), palladium nitrate (Pd (NO 3 ) 2 ), palladium sulfate (PdSO 4 ), potassium tetrachloropalladate (K 2 (PdCl 4 )), potassium tetrabromopalladate (K 2 (PdBr 4 )) , Tetraammine palladium chloride (Pd (NH 3 ) 4 Cl 2 ), tetraammine palladium bromide (Pd (NH 3 ) 4 Br 2 ), tetraammine palladium nitrate (Pd (NH 3 ) 4 (NO 3 ) 2 ), tetraammine palladium tetra
  • the noble metal precursors may be used alone or in combination of two or more.
  • the amount used is usually 0.01 parts by mass or more in terms of the amount of photocatalyst particles used in terms of 100 parts by mass in terms of noble metal atoms, and usually 1 part by mass or less in that an effect commensurate with the cost is obtained. It is.
  • the amount of the noble metal precursor used is 0.05 to 0.6 parts by mass, more preferably, with respect to 100 parts by mass of the photocatalyst particles in terms of noble metal atoms. 0.05 to 0.2 parts by mass.
  • the amount of the precursor of the noble metal converted to a noble metal atom is not less than 0.01 parts by mass with respect to the amount of photocatalyst particles used of 100 parts by mass.
  • the virus titer of a virus having an envelope and not having an envelope can be reduced by 1.5 (Log 10 TCID 50 / ml) or more, and such a virus can be inactivated.
  • the photocatalyst particle dispersion in which the precursor of the noble metal is dissolved is used as a raw material dispersion.
  • a sacrificial agent is added to the raw material dispersion.
  • the sacrificial agent include alcohols such as ethanol, methanol, and propanol, ketones such as acetone, and carboxylic acids such as oxalic acid.
  • the sacrificial agent may be used by dissolving in a suitable solvent, or may be used as a solid.
  • the sacrificial agent is added to the raw material dispersion after light irradiation for a certain period of time, and further light irradiation is performed.
  • the amount of the sacrificial agent is usually 0.001 to 0.3 times by mass, preferably 0.005 to 0.1 times by mass with respect to the dispersion medium. If the amount of the sacrificial agent used is less than 0.001 times by mass, the noble metal is insufficiently supported on the photocatalyst particles, and if it exceeds 0.3 times by mass, the amount of sacrificial agent is excessive and an effect commensurate with the cost cannot be obtained. .
  • the raw material dispersion is irradiated with light.
  • You may perform irradiation of the light to a raw material dispersion liquid, stirring. Irradiation may be performed from inside or outside the tube while passing the raw material dispersion through a transparent glass or plastic tube, or this may be repeated.
  • the light source is not particularly limited as long as it can irradiate light having energy higher than the band gap of the photocatalyst particles, and specific examples include germicidal lamps, mercury lamps, light emitting diodes, fluorescent lamps, halogen lamps, xenon lamps, solar Light can be used.
  • the wavelength of the irradiated light is usually 180 nm to 500 nm.
  • the light irradiation time is usually 20 minutes or longer, preferably 1 hour or longer, and usually 24 hours or shorter, preferably 6 hours or shorter, before and after the addition of the sacrificial agent.
  • the time exceeds 24 hours, most of the precursors of the noble metal have been supported as noble metals by that time, and an effect commensurate with the cost of light irradiation cannot be obtained.
  • the precious metal is not uniformly supported, and high antiviral activity cannot be obtained.
  • PH adjustment In the present invention, light irradiation is performed while maintaining the pH of the raw material dispersion at 2.5 to 4.5, preferably 2.8 to 4.0.
  • the pH of the dispersion gradually changes to acidic, so that a base is usually added to maintain the pH within the range specified in the present invention. do it. Thereby, a noble metal-supported photocatalyst dispersion with excellent dispersibility is obtained.
  • Examples of the base include aqueous solutions of ammonia, sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, lanthanum hydroxide, etc. Among them, ammonia and sodium hydroxide are used. It is preferable to use it.
  • the amount of dissolved oxygen in the raw material dispersion is adjusted to 1.0 mg / L or less, preferably 0.7 mg / L or less as necessary.
  • the amount of dissolved oxygen can be adjusted, for example, by blowing a gas containing no oxygen into the raw material dispersion, and examples of the gas include nitrogen and rare gases (helium, neon, argon, krypton, etc.). .
  • the amount of dissolved oxygen exceeds 1.0 mg / L, a reduction reaction of dissolved oxygen occurs in addition to the loading of the precursor of the noble metal, the loading of the noble metal becomes uneven, and high antiviral activity cannot be obtained.
  • the amount of dissolved oxygen is reduced to a predetermined value or less, light irradiation is performed, and after addition of the sacrificial agent, the light is further irradiated, so that the noble metal precursor becomes a noble metal, which becomes the photocatalyst particles.
  • Noble metal-supported photocatalyst particles are obtained by being supported on the surface.
  • the noble metal-supported photocatalyst particles are dispersed in the used dispersion medium without settling. Further, the dispersion liquid in which the noble metal-supported photocatalyst particles are dispersed is easy to handle because of the excellent dispersibility of the noble metal-supported photocatalyst particles, and also exhibits high antiviral activity.
  • the photocatalyst particles of the present invention are 4.0 ⁇ 10 17 or more, preferably 6.0 ⁇ 10 17 per 1 g of photocatalyst particles when irradiated with visible light in a dispersion state in which the photocatalyst particles are dispersed in water. As described above, more preferably 7.5 ⁇ 10 17 or more OH radicals are generated. When the amount of OH radicals produced is less than 4.0 ⁇ 10 17 , sufficient antiviral properties cannot be obtained under visible light irradiation. Therefore, when the amount of OH radicals produced is 4.0 ⁇ 10 17 or more, sufficient antiviral properties can be obtained under irradiation with visible light.
  • the amount of radical generated is determined by observing the ESR spectrum after irradiating the noble metal-supported photocatalyst dispersion with visible light in the presence of DMPO (5,5-dimethyl-1-pyrroline-N-oxide), which is a radical scavenger. Then, an area value of a signal is obtained for the obtained spectrum and calculated from the area value.
  • DMPO 5,5-dimethyl-1-pyrroline-N-oxide
  • irradiation with visible light is performed at room temperature and in the atmosphere for 20 minutes using a white light emitting diode as a light source and an illuminance of 20000 lux.
  • the measurement of the ESR spectrum is performed in a state in which the light from a fluorescent lamp having an illuminance of less than 500 lux is irradiated as room light using EMX-Plus (manufactured by BRUKER) after irradiation with visible light for 20 minutes.
  • the measurement conditions of the ESR spectrum are as follows. Temperature: Room temperature, Pressure: Atmospheric pressure, Microwave Frequncy: 9.86GHz, Microwave Power: 3.99mW, Center Field: 3515G, Sweep Width: 100G, Conv.
  • the ESR spectrum of DMPO-OH which is an OH radical adduct of DMPO, is compared with the ESR spectrum of a substance having a known number of radicals.
  • a relational expression between the area obtained from the ESR spectrum and the number of radical species is obtained by the following procedure.
  • 4-hydroxy-TEMPO is used as a substance with a known radical number.
  • 0.17621 g of 4-hydroxy-TEMPO (4-Hydroxy-2,2,6,6-tetramethyl-piperidine-1-oxyl) (purity 98%) is dissolved in 100 mL of water.
  • the liquid obtained is designated as A.
  • B Take 1 mL of B and add water to make 100 mL.
  • C be the resulting liquid.
  • the concentration is 0.001 mM.
  • the number y1 of OH radicals after irradiation with the white light-emitting diode is calculated from the ESR spectrum of DMPO-OH and the first-order linear approximation calculated using the known concentration of 4-hydroxy-TEMPO. Further, the number of OH radicals y2 contained in the noble metal-supported photocatalyst dispersion before light irradiation is calculated in the same manner, and the difference (y1-y2) is the number of OH radicals generated by irradiation of the white light emitting diode.
  • the photocatalyst particle dispersion or the noble metal-supported photocatalyst dispersion used in the present invention may contain various known additives as long as the effects of the present invention are not impaired.
  • additives include silicon compounds such as amorphous silica, silica sol, water glass, alkoxysilane, and organopolysiloxane, aluminum compounds such as amorphous alumina, alumina sol, and aluminum hydroxide, and aluminosilicates such as zeolite and kaolinite.
  • Alkaline earth metal oxides such as salts, magnesium oxide, calcium oxide, strontium oxide, barium oxide, alkaline earth metal hydroxides such as magnesium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, Ti, Zr , Hf, V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, Fe, Co, Ni, Ru, Rh, Os, Ir, Ag, Zn, Cd, Ga, In, Tl, Ge, Sn , Pb, Bi, La, Ce and other metal element hydroxides and oxides, zirco oxalate Um, calcium phosphate, molecular sieve, active carbon, a polycondensation product of an organopolysiloxane compound, phosphate, a fluorine-based polymer, silicone-based polymers, acrylic resins, polyester resins, melamine resins, urethane resins, alkyd resins. When these additives are added and used, they can be used alone or in
  • the additive can also be used as a binder for holding the photocatalyst particles more firmly on the surface of the substrate when the photocatalyst layer is formed on the surface of the substrate using the photocatalyst.
  • binder component for the photocatalyst layer examples include zirconium compounds such as zirconium formate, zirconium glycolate, zirconium oxalate, zirconium hydroxide and zirconium oxide; tin compounds such as tin hydroxide and tin oxide; niobium hydroxide and oxide Niobium compounds such as niobium; silicon alkoxides such as tetraethoxysilane (ethyl silicate), tetramethoxysilane (methyl silicate), methyltriethoxysilane, and methyltriethoxysilane; silicon compounds such as colloidal silica and silicon oxide These can be used alone or in combination of two or more.
  • the amount of the binder component contained in the photocatalyst layer is 3 to 40 parts by mass, preferably 4 to 20 parts by mass in terms of oxide with respect to 100 parts by mass of the photocatalyst layer.
  • the amount of the binder is less than 3 parts by mass, the force for holding the photocatalyst particles in the photocatalyst layer becomes weak, and problems such as the photocatalyst particles falling off easily occur.
  • the amount of the binder exceeds 40 parts by mass, the amount of the binder component that covers the surface of the photocatalyst particles increases, and sufficient antiviral performance cannot be obtained.
  • the photocatalyst structure used in the present invention comprises a photocatalyst layer on the surface, and usually comprises a photocatalyst layer on the substrate surface.
  • the photocatalyst layer is prepared by a conventionally known film-forming method such as mixing the noble metal-supported photocatalyst particle dispersion and a binder, applying this to the surface of the substrate (product), and volatilizing the dispersion medium. Can be formed.
  • the film thickness of the photocatalyst body layer is not particularly limited, and may usually be appropriately set in the range of several tens of nanometers to several millimeters according to the application.
  • the photocatalyst layer may be formed on any part as long as it is an inner surface or an outer surface of the base material (product).
  • the photocatalyst layer is a surface irradiated with light (visible light) and a virus It is preferably formed on a surface that is continuously or intermittently connected to an existing location.
  • the material of the base material is not particularly limited as long as the formed photocatalyst layer can be held with sufficient strength to be practically used.
  • any material such as plastic, metal, ceramics, wood, concrete, paper, etc. It can target products consisting of
  • antiviral agents can be used for building materials such as ceiling materials, tiles, glass, wallpaper, wall materials, films, floors, etc., automotive interior materials (automobile instrument panels, automotive seats, automotive ceiling materials, automotive products).
  • Parvovirus B19 of the family Parvoviridae, cat parvo which is a virus with a size of 15 to 30 nm and no envelope when used as a base material that can be contacted by an unspecified number of people, such as straps, elevator buttons, etc.
  • Viruses canine parvovirus, goose parvovirus, swine parvovirus, picornaviridae poliovirus, Telovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, aichivirus, Astroviridae human astrovirus, ubiastrovirus, It can inactivate turkey astrovirus, duck astrovirus, porcine circovirus of the circoviridae, chicken anemia virus, torque tenovirus (TT virus).
  • TT virus torque tenovirus
  • BET specific surface area The BET specific surface area of the photocatalyst particles was measured by a nitrogen adsorption method using a specific surface area measuring device (“Monosorb” manufactured by Yuasa Ionics).
  • Average dispersed particle size (nm) The particle size distribution was measured using a submicron particle size distribution measuring device (“N4Plus” manufactured by Coulter, Inc.), and the result obtained by automatically performing the monodisperse mode analysis with the software attached to this device was used as the average dispersed particle size. .
  • Crystalline X-ray diffraction spectrum was measured using an X-ray diffractometer (“RINT2000 / PC” manufactured by Rigaku Corporation), and the crystal form was determined from the spectrum.
  • Dissolved oxygen The dissolved oxygen in the raw material dispersion was measured using a dissolved oxygen meter ("OM-51" manufactured by Horiba, Ltd.).
  • Antiviral properties were evaluated by measuring the virus titer of goose parvovirus by irradiation with visible light from a fluorescent lamp. That is, spin coater (“1H-Mikasa” manufactured by Mikasa Co., Ltd.) was applied to a glass plate (5 cm ⁇ 5 cm ⁇ 2 mm) so that the obtained photocatalyst coating liquid was 1 g / m 2 in terms of solid content conversion per unit area. D7 ”) and uniformly formed on one side of the glass plate. Next, this glass plate was dried by holding it in the air at 130 ° C. for 10 minutes in the air, thereby forming a photocatalyst layer on one side of the glass plate.
  • the photocatalyst layer has an ultraviolet intensity of 2 mW / cm 2 (measured by attaching a UV receiver “UD-36” to Topcon's UV intensity meter “UVR-2”). This was irradiated for a period of time and used as a sample for measuring antiviral activity.
  • GPV-IHC (DE15DEF25 2011/2/23) was used for the goose parvovirus. That is, inoculate the photocatalyst layer with a test solution containing a virus, put a coating film on the photocatalyst layer, and make a close contact, and store it at room temperature (25 ⁇ 5 ° C.) under visible light irradiation or shading for 6 hours.
  • the virus titer was determined as the logarithmic value (Log TCID 50 / ml) of 50% tissue culture infectious amount using Muscovy duck embryo fibroblast (MDEF).
  • a test solution containing virus and MDEF were prepared in the following maintenance medium (MM) or growth medium (GM).
  • MM maintenance medium
  • FBS fetal bovine serum
  • GM growth medium
  • CPE cytopathic effect
  • the recovered virus solution was transferred to a microtube, treated with a centrifuge at 15000 rpm for 3 minutes, and the titer of the remaining virus was measured on the supernatant.
  • the virus titer was measured by inoculating a 96-well tissue culture plate with 4 wells of each diluted dilution of the virus solution 10 times with MM. Before inoculation, GM was removed from MDEF, and 100 ⁇ l of diluted virus solution was inoculated therein. The CPE at 7 days after the inoculation was observed, and the virus titer (50% tissue culture infectious dose per ml: TCID 50 / ml) was calculated from the number of positive holes at each dilution by the Behrens Kerber method. )
  • Evaluation of antiviral property was performed simultaneously using three samples for measuring antiviral activity, and the evaluation was performed using the average value of logarithmic values of these three virus titers.
  • Irradiation with visible light uses a commercially available white fluorescent lamp (20 W, 2) as a light source, and is included in the fluorescent lamp from above the photocatalyst layer on which the coating film is placed through an acrylic resin plate (“N113” manufactured by Nitto Resin Kogyo). The visible light was irradiated. At this time, irradiation in the vicinity of the coating film was set to 1000 lux (measured by Minolta “T-10”).
  • the measurement limit of the logarithmic value of the virus titer was 1.5.
  • Example 1 1 kg of tungsten oxide particles (manufactured by Nippon Inorganic Chemical Co., Ltd.) was added to 4 kg of ion exchange water as a dispersion medium and mixed to obtain a mixture. This mixture was dispersed using a wet medium stirring mill to obtain a tungsten oxide particle dispersion.
  • the average dispersed particle diameter of the tungsten oxide particles in the obtained tungsten oxide particle dispersion was 118 nm. Moreover, when a part of this dispersion was vacuum-dried to obtain a solid content, the BET specific surface area of the obtained solid content was 40 m 2 / g.
  • the mixture before dispersion treatment was similarly vacuum dried to obtain a solid content, and the solid content of the mixture before dispersion treatment and the solid content after dispersion treatment were measured and compared with each other, The peak shape was the same, and no change in crystal form due to dispersion treatment was observed. At this time, when the obtained dispersion was kept at 20 ° C. for 24 hours, no solid-liquid separation was observed during storage.
  • tungsten oxide particle dispersion To this tungsten oxide particle dispersion, an aqueous solution of hexachloroplatinic acid (H 2 PtCl 6 ) is added so that hexachloroplatinic acid is 0.12 parts by mass with respect to 100 parts by mass of tungsten oxide particles in terms of platinum atoms, A hexachloroplatinic acid-containing tungsten oxide particle dispersion was obtained as a raw material dispersion.
  • the solid content (amount of tungsten oxide particles) contained in 100 parts by mass of this dispersion was 17.6 parts by mass (solid content concentration 17.6% by mass).
  • This is a light irradiation device consisting of a glass tube (inner diameter: 37 mm, height: 360 mm) with an underwater sterilization lamp (manufactured by Sankyo Electric Co., Ltd., GLD15MQ), and while distributing 1200 g of the raw material dispersion at a rate of 1 liter per minute, The pH of the dispersion was adjusted to 3.0. Nitrogen was blown at a rate of 2 L / min.
  • 83.28 g of high purity ethyl silicate (manufactured by Tama Chemical) was added to a solution obtained by mixing 86.52 g of ethanol with 30.2 g of water, and mixed and stirred to obtain a binder for a photocatalyst layer.
  • the amount of the binder component contained in the photocatalyst layer obtained from this photocatalyst coating liquid was 5 parts by mass with respect to 100 parts by mass of the photocatalyst layer in terms of oxide.
  • the virus titer against goose parvovirus that was 4.2 (Log 10 TCID 50 / ml) when the light irradiation time was 0 hour was 1.5 (Log 10 TCID 50 / ml) (below detection limit).
  • Viral titer decreased over 2.7.
  • Example 1 When antiviral properties were evaluated in the same manner as in Example 1 except that raw glass without a photocatalyst layer was used, the goose was 4.2 when the light irradiation time was 0 hour. The virus titer against parvovirus was 3.9 after 6 hours of light irradiation. The decrease in virus titer was 0.3.
  • parvovirus B19 By using the antiviral agent obtained in Example 1 as a ceiling material constituting the ceiling, parvovirus B19, cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus in indoor space by light irradiation with indoor lighting.
  • Poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, aichi virus, human astrovirus, siastrovirus, turkey Astroviruses, duck astroviruses, porcine circoviruses, and chicken anemia viruses can be inactivated.
  • parvovirus B19 By using the antiviral agent obtained in Example 1 on an indoor wall surface, parvovirus B19, cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus in indoor space by light irradiation with indoor lighting.
  • Enterovirus human bar echo virus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, aichi virus, human astrovirus, ubiastrovirus, turkey astrovirus, It can inactivate duck astrovirus, porcine circovirus and chicken anemia virus.
  • B19 cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis B virus, It can inactivate swine tesovirus, aichi virus, human astrovirus, usciatrovirus, turkey astrovirus, duck astrovirus, porcine circovirus and chicken anemia virus.
  • a photocatalyst layer can be formed on the surface of the wallpaper.
  • Parvovirus B19 cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echo virus, human rhinovirus A to B, A type in indoor space by light irradiation by indoor lighting Inactivate hepatitis virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, eye virus, human astrovirus, siastrovirus, turkey astrovirus, duck astrovirus, porcine circovirus, chicken anemia virus Can do.
  • the antiviral agent obtained in Example 1 can be used on an indoor floor surface or applied to the floor surface to form a photocatalyst layer on the floor surface.
  • Parvovirus B19 cat parvovirus, canine parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus in indoor space , Equine rhinitis B virus, swine teshovirus, ichi virus, human astrovirus, ussia trovirus, turkey astrovirus, duck astrovirus, porcine circovirus, chicken anemia virus can be inactivated.
  • Example 6 By applying the antiviral agent obtained in Example 1 to the surface of an automotive interior material such as an automotive instrument panel, an automotive seat, an automotive ceiling material, or the interior of an automotive glass, It is possible to form a photocatalyst layer on the surface, and thereby, in the interior space by light irradiation by interior illumination, parvovirus B19, cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, Human bar echo virus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, eye virus, human astrovirus, siastrovirus, turkey astrovirus, duck astrovirus , Porcine circovirus, chicken Capable of inactivating the blood virus.
  • parvovirus B19 cat parvovirus
  • dog parvovirus dog parvovirus
  • goose parvovirus swine parvovirus
  • Parvovirus B19 cat parvovirus
  • Parvovirus B19 cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, horse It can inactivate rhinitis B virus, swine tesovirus, ichi virus, human astrovirus, ussia trovirus, turkey astrovirus, duck astrovirus, porcine circovirus and chicken anemia virus.
  • parvovirus B19 cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus on the surface of the base material by light irradiation with indoor lighting.
  • Virus A to B Hepatitis A virus, Encephalomyocarditis virus, Equine rhinitis virus B, Swine teshovirus, Aichi virus, Human astrovirus, Ussia trovirus, Turkey astrovirus, Duck astrovirus, Porcine circovirus, Chicken anemia Viruses can be inactivated.
  • a photocatalyst layer can be formed on the substrate surface, Parvovirus B19, cat parvovirus, canine parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus A to B, A on the surface of the substrate by light irradiation with indoor lighting Inactivate hepatitis B virus, encephalomyocarditis virus, equine rhinitis B virus, swine teshovirus, aichi virus, human astrovirus, ussia trovirus, turkey astrovirus, duck astrovirus, porcine circovirus, chicken anemia virus be able to.
  • Example 11 By providing or affixing the antiviral agent obtained in Example 1 on the surface of home appliances such as personal computers, printers, scanners, copiers, fax machines, telephones, televisions, stereos, washing machines, stoves, dryers, microwave ovens, etc.
  • a photocatalyst layer can be formed on the surface of the base material, whereby parvovirus B19, cat parvovirus, dog parvovirus, goose parvovirus, swine parvovirus on the base material surface by light irradiation with indoor lighting.
  • Poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, encephalomyocarditis virus, equine rhinitis virus B, swine teshovirus, aichi virus, human astrovirus, siastrovirus, turkey Astrovirus, duck ass B virus, porcine circovirus, a chicken anemia virus may be inactivated.
  • a photocatalyst layer By applying and drying the antiviral agent obtained in Example 1 on the surface of cocoons, tatami mats, shoji, etc., a photocatalyst layer can be formed on the surface of the base material.
  • the parvovirus B19 cat parvovirus
  • canine parvovirus canine parvovirus, goose parvovirus, swine parvovirus, poliovirus, enterovirus, human bar echovirus, human rhinovirus AB, hepatitis A virus, brain It can inactivate myocarditis virus, equine rhinitis B virus, swine teshovirus, ichi virus, human astrovirus, ussia trovirus, turkey astrovirus, duck astrovirus, porcine circovirus and chicken anemia virus.
  • a photocatalyst layer By forming or sticking the antiviral agent obtained in Example 1 on the surface of the film, a photocatalyst layer can be formed on the surface of the film, and this film can be used as a building material, furniture, wall, floor, ceiling, Parvovirus B19, cat parvovirus, dog parvovirus on the surface of the film by irradiating light with indoor lighting by constructing it on the touch panel, equipment buttons, doors, door knobs, handrails of stairs, interior walls of aircraft and train cabins, etc.

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Abstract

L'invention concerne : un agent antiviral qui peut présenter une activité antivirale élevée même sous l'irradiation par de la lumière visible et peut inactiver un virus ; et un procédé d'inactivation d'un virus. L'invention concerne un agent antiviral contenant une structure photocatalyseur qui présente, formée sur la surface de celle-ci, une couche photocatalyseur comprenant des particules de photocatalyseur sur lesquelles des particules de métal noble sont supportées, et un liant, l'agent antiviral étant caractérisé en ce que les particules de métal noble sont supportées dans une quantité de 0,01 à 1 partie en masse par rapport à 100 parties en masse des particules de photocatalyseur et l'agent antiviral peut inactiver un virus ayant une dimension de 15 à 30 nm et n'ayant pas d'enveloppe.
PCT/JP2012/067559 2011-07-11 2012-07-10 Agent antiviral apte à inactiver un virus, et procédé d'inactivation d'un virus WO2013008807A1 (fr)

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JP2013067577A (ja) * 2011-09-21 2013-04-18 Nbc Meshtec Inc 抗ウイルス剤およびそれを用いた部材
JP2015059089A (ja) * 2013-09-17 2015-03-30 昭和電工株式会社 抗ウイルス性組成物、その製造方法およびウイルス不活性化方法
JP5673782B1 (ja) 2013-11-11 2015-02-18 凸版印刷株式会社 液晶表示装置

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JP2011050802A (ja) * 2009-01-27 2011-03-17 Sumitomo Chemical Co Ltd 貴金属担持光触媒体粒子分散液の製造方法
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