WO1997000134A1 - Photocatalyst-carrying structure and photocatalyst coating material - Google Patents
Photocatalyst-carrying structure and photocatalyst coating material Download PDFInfo
- Publication number
- WO1997000134A1 WO1997000134A1 PCT/JP1996/001669 JP9601669W WO9700134A1 WO 1997000134 A1 WO1997000134 A1 WO 1997000134A1 JP 9601669 W JP9601669 W JP 9601669W WO 9700134 A1 WO9700134 A1 WO 9700134A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- photocatalyst
- layer
- adhesive layer
- silicon
- resin
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/477—Titanium oxide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/478—Silica
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/71—Photocatalytic coatings
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/256—Heavy metal or aluminum or compound thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/256—Heavy metal or aluminum or compound thereof
- Y10T428/257—Iron oxide or aluminum oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/258—Alkali metal or alkaline earth metal or compound thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/259—Silicic material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31609—Particulate metal or metal compound-containing
- Y10T428/31612—As silicone, silane or siloxane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31667—Next to addition polymer from unsaturated monomers, or aldehyde or ketone condensation product
Definitions
- a photocatalyst coating solution that does not increase in viscosity or settle particles even after storage for at least one month, or preferably for three months or more, is required. is necessary. It is also necessary to support photocatalyst without impairing the photocatalytic action when coated on practical products.
- the adhesive layer be made of a silicone-modified resin such as an acrylic-silicon resin or an epoxy-silicon resin having a silicon content of 2 to 60% by weight, or colloidal silica. Resin containing up to 40% by weight, or general formula (1)
- the photocatalyst supporting structure and the photocatalyst coating agent can be supported on a carrier material such as glass, plastic, metal, cloth, or wood material, and can be used for a lens, an adhesive film, a blind, It has been found that the photocatalyst coating agent according to the present invention can be applied to nonwoven fabrics, wooden doors, and the like.
- an acrylic resin or an epoxy resin is the most excellent in terms of film formability, toughness, and adhesion to a carrier, but an alkyd resin, a urethane resin, Materials such as polyester resins can also be used. These resins can be used either as a type dissolved in a solvent or as an emulsion type. There is no problem even if additives such as a crosslinking agent are included.
- the particle diameter of the colloidal silica is preferably 10 nm or less. If the thickness exceeds 10 nm, the resin in the adhesive layer is not only easily deteriorated by the photocatalyst, but also the adhesion between the photocatalyst layer and the adhesive layer is deteriorated.
- the simplest way to introduce this colloidal silicide into the resin is to mix the resin solution with the colloidal silicide solution, then apply and dry to form an adhesive layer. In a dispersed state, the resin may be polymerized and synthesized, applied and dried before use. Further, in order to improve the adhesion and dispersibility between the colloidal silica and the resin, the colloidal silica may be treated with a silane coupling agent before use.
- any powder, sol, solution or the like that can exhibit photocatalytic activity by being fixed to the adhesive layer when dried at the drying temperature of the photocatalytic layer can be used.
- a sol-shaped photocatalyst if the particle size is 2 O nm or less, preferably 1 O nm or less, the transparency of the photocatalyst layer is improved, and the linear transmittance is increased. It is particularly preferable when applied to a required glass substrate or plastic molded body. Further, in the case where a color or pattern is printed on the underlying carrier, applying such a transparent photocatalyst layer does not impair the underlying color or pattern.
- the silicone compound to be added to the coating solution for the photocatalyst layer of the present invention is represented by the general formula (2)
- a method for adding the silicon compound to the coating solution for the photocatalyst layer a method for adding the silicon compound to the solution of the photocatalyst powder or the sol, a method for adding a metal oxide and / or a metal oxide to be added together with the photocatalyst are used.
- Various methods such as a method of adding a hydroxide sol to a liquid are possible.
- a partially hydrolyzed silicone compound may be added.
- the silicon compound added to the coating solution for the photocatalyst layer also has the effect of enhancing the adhesion of the photocatalyst layer in boiling water. Therefore, when the above-mentioned silane coupling agent or the like is added, the silicon compound is used.
- a product exhibiting excellent weather resistance such that the adhesion of the ISK550 by the grid tape method maintains an evaluation score of 6 or more is also obtained. Furthermore, after being immersed in boiling water having a conductivity of 200 ⁇ S cm at 20 ° C. for 15 minutes, the adhesion by the cross-cut tape method specified in JISK 540 was evaluated 6 points. A product exhibiting the above high boiling water resistance can be obtained, and all of the samples exhibit high photocatalytic activity. .
- the glass provided with the adhesive layer and the photocatalyst layer can be obtained even in a complicated shape such as a rectangular shape, a tubular shape, a spherical shape, or a fibrous shape. Also, if the size is 1 Qm or more, it can be firmly supported. In addition, depending on applications such as constructed window glass, showcases, and glasses, the processed glass can be processed into the photocatalyst-supporting glass of the present invention.
- the glass supporting the photocatalyst according to the present invention includes antibacterial agents such as window glass, cover glass for instruments, lighting equipment, lighting, black light, fillers for water treatment, cameras, eyeglass lenses, and the like. It can be used in any situation where effects such as deodorization and antifouling are required.
- the plastic molded article carrying the photocatalyst according to the present invention has effects such as antibacterial, deodorizing, and antifouling effects such as wallpaper, interior boards, furniture, electric equipment, and vehicle parts, as well as camera and bead lenses. It can be used in many situations where
- Fabric, water-repellent fabric that uses a cross-linking agent such as ethylenimine, epoxy, or melamine to improve durability, if necessary.
- Synthetic leather or the like in which a polyurethane resin layer is formed on a base material such as artificial leather, woven fabric, non-woven fabric, or knitted fabric made of fibrilated conjugate fiber, etc. via a polyurethane adhesive. It can also be used.
- the photocatalyst-carrying fabric of the present invention can be obtained by treating a processed fabric such as an umbrella, a tent, a bag, or the like.
- the fabric carrying the photocatalyst according to the present invention can be used in many applications where effects such as antibacterial, deodorizing, and antifouling are required, for example, intellectual products such as power and wallpaper, tents, umbrellas, and table cloths It can be used as a daily necessity, food packaging material, etc., and also in the agricultural field such as a nursery sheet.
- the metal supporting the photocatalyst according to the present invention includes window frames, furniture, decorative articles, interior panels, exterior panels, fillers for water treatment, strainers, filters, etc., antibacterial, deodorizing, antifouling, etc. It can be used in many usage situations that require the effect of.
- the shape of the wood or woody material provided with the adhesive layer and the photocatalyst layer according to the present invention can be any complicated shape such as a plate, a plate, a sphere, a sheet, and the like.
- the size is 10 m or more, it can be firmly supported, and it should be processed into processed walls and ceiling panels, pillars, furniture and woodwork, and other processed wood and wood materials. Thereby, the photocatalyst-carrying wood and woody material of the present invention can be obtained.
- the photocatalyst-supporting wood and wood-based materials shown in the present invention are used in many usage situations requiring antibacterial, deodorizing, and antifouling effects, such as building materials, furniture, woodwork, interior materials, and interior materials. it can.
- the plastic film provided with the photocatalyst supporting structure according to the present invention makes use of its antifouling, antibacterial, and deodorizing functions to form a film in which an adhesive is applied to a surface that does not support the photocatalyst.
- a thin plastic film in which the photocatalyst supporting structure according to the present invention is formed into a film can be used as a wrap film for food packaging.
- the resins that can be used for this plastic film include polyethylene terephthalate resin, polycarbonate resin, polyacrylate resin, polymethyl methacrylate resin, polyethylene resin, polypropylene resin, and polyamide resin. 550 nm when formed into a film such as polyimide resin, polyimide resin, polystyrene resin, polyvinyl chloride resin, polyvinylidene fluoride resin, fluorinated ethylene-propylene copolymer resin, fluorinated ethylene-ethylene copolymer resin, etc.
- Highly transparent synthetic resin film with a linear transmittance of 50% or more for light of You can use either a room or a seat.
- the photocatalyst supporting structure according to the present invention is transparent even on the surface of an opaque material with a sticky layer and a release film on the back surface such as a wallpaper or decorative sheet and a pattern printed on the surface. It can be used favorably because it does not damage the pattern or pattern printed on the wallpaper or decorative sheet.
- the surface of these synthetic resin films or sheets can be subjected to a surface treatment to further improve the adhesiveness of the adhesive layer of the photocatalyst supporting structure, and the surface to which the adhesive layer is applied can be subjected to corona discharge treatment or UV irradiation. It is also possible to favorably use a material in which the surface is physically oxidized in a trace amount by ozone treatment or the like and a surface treatment agent such as a silicon-based material is thinly applied to improve the familiarity with the adhesive layer. Furthermore, as shown in the examples, a thin film for heat ray reflection / shielding function or ultraviolet ray reflection / shielding function can be provided on the front surface or the back surface of these substrates.
- a heat ray S film having both antifouling, antibacterial, and deodorizing functions can be used as a UV ray film, and the photocatalyst supporting structure according to the present invention has extremely high durability as shown in the examples. Since it has both properties and photocatalytic activity, it can be a product with extremely high added value.
- Methods for providing the above-described heat ray reflection function include conductive metals such as Al, Ag, Cii, Cr, Ni, Ti, stainless steel, and aluminum alloy, indium oxide, tin oxide, and the like.
- a method of depositing a conductive metal oxide such as tin oxide monoxide on a film surface by physical methods such as sputtering or vacuum deposition, and applying a conductive metal oxide solution or a sol solution Various methods can be adopted, such as a method of drying, forming a film on the film surface by plating method or CVD method, and a method of mixing materials having heat ray reflection properties and heat ray shielding properties into the resin of the base material. is there.
- a method of providing an ultraviolet ray shielding function there is a method of applying a UV absorbent or a reflective agent such as a hindered amine-based titanium oxide to the surface of the film to form a film, and the UV absorbent is used in advance.
- a method of adding and mixing with a film base can be adopted, and an appropriate method can be selected according to a use purpose and a structure.
- titanium oxide is used as an ultraviolet shielding agent or a reflective agent, as described in detail in the present invention, the use of titanium oxide alone decomposes surrounding organic substances by the action of a photocatalyst. Surface with water glass etc. It is desirable to use a thin coating with no photocatalytic activity.
- such a material having a heat ray reflecting function or a material having an ultraviolet ray shielding function can be added to and mixed with an adhesive layer formed on the back surface of the film to exert the effect.
- Materials such as an ultraviolet shielding clear coating agent described in the March 2006 issue, pp 95, are solvent-dispersible and can be used.
- Adhesives such as acrylic-based and silicon-based are usually used as the adhesive, but various ultraviolet shielding agents and heat ray shielding agents can be added to the adhesive. It is desirable to avoid using a pressure-sensitive adhesive having strong adhesiveness in consideration of contamination due to residual adhesion of the pressure-sensitive adhesive at the time of replacement.
- FIG. 1 is a schematic view of a cross section of a photocatalyst supporting structure of the present invention.
- the accelerated weathering test using a sunshine carbon arc weather meter specified in JISK 540 was carried out using a WE L—S UN—HCH type manufactured by Suga Test Instruments Co., Ltd. for a test time of 500 Time, black panel temperature 63 C, 120 min cycle, 18 min rainfall conditions. After subjecting three samples to the accelerated weathering test, the presence or absence of blisters, cracks, peeling, and whitening, and changes in the surface are visually compared with the original test specimens that are not subjected to the accelerated weathering test. Was evaluated.
- Antibacterial evaluation test method-A sample cut into 5 cm squares is disinfected with 80% ethanol, dried at 150 ° C, sterilized, and pre-cultured and diluted beforehand to reduce the bacterial concentration to 10%.
- Five (0.2) ml of the bacterial solution of E. coli adjusted to Zm 1 is dropped on the sample surface, and set in the incubator.
- a commercial salad oil containing linoleic acid as the main component was used to measure how quickly oils and fats attached to the surface can be decomposed on the photocatalyst structure.
- the amount of decomposition was determined.
- Salad oil was thinly coated with paper on the surface of the photocatalyst-supporting structure cut into a square of 5 cm at a concentration of 0.1 to 0.15 mg / cm 2 .
- the amount of coating was determined by measuring the weight before and after coating with a precision balance.
- Samples were adjusted to the distance between the sample and the black line Bok as an ultraviolet intensity at the sample surface is 3 mW / cm 2, after lighting the black line bets, seeking relationship elapsed time and the weight loss, the predetermined time period The decomposition amount of the salad oil afterwards was measured and used as an index for antifouling property.
- the adhesive layer was formed by a diving method when the thickness was 2 m or less or in a shape other than a flat plate, and was formed by a baili force applicator when the thickness was 2 m or more and in a flat plate shape. In particular, when the shape of the carrier was tubular or net-like, the diving method was used. Drying of the adhesive layer was carried out at 80 ° C. for the carrier material (T E) and (T F), at 60 ° C. for (T B), and at 120 ° C. for other cases. The following were used as the photocatalyst.
- C-1 titanium oxide fine particles (trade name P-25, manufactured by Nippon Aerosil Co., Ltd., crystal particle diameter 27 nm)
- Titanium oxide sol (acid sol of nitric acid, crystal particle diameter 1 O nm)
- ZR ZR is hydrolyzed in ethanol, dried at 150 ° C, heat-treated at 300 to 50 ° C, and peptized with dilute aqueous nitric acid solution. Specific surface area of dried at 50 ° C is 50 to 80 m2 / g
- Niobium oxide sol An aqueous solution of niobium oxalate manufactured by CBMM was neutralized with 10% ammonia water, dried at 150 ° C and peptized with a dilute aqueous nitric acid solution. The specific surface area of the product dried at 50 is 60 m2 / g
- a titanium oxide photocatalyst was dispersed in the above solution, and a predetermined amount of a surfactant was added to obtain a solution for forming a photocatalyst layer.
- the photocatalyst layer was formed by a diving method when the thickness was 2 or less or the carrier shape was other than a flat plate, and was formed by a bar coater when the carrier was a flat plate and the thickness was 2 or more.
- the drying of the photocatalyst layer was performed at the same temperature as the drying of the adhesive layer.
- Comparative Example-1 shows a case where the photocatalyst layer was carried without providing an adhesive layer, and there was no adhesion of the photocatalyst layer, and it was easily peeled off, and the polyester film after the durability test. The surface of the lum was degraded by photocatalysis, and holes and cracks were observed.
- Examples 1-1 and --2 an acrylic silicon resin or a polyester-silicon resin was used for the adhesive layer.
- the adhesion of the photocatalyst layer was good, and the durability was also good. .
- Example 11 In Examples 11 to 18, titanium oxide (P-25) manufactured by Japan Air Gill Co., Ltd. shown in (C-11) was used as a photocatalyst, and a metal oxide compounded in the photocatalyst layer was used. Most of the sols or metal hydroxide sols use silica sol, but all are good 4 things have been obtained. In Examples 18 and 19, the results of carrying on a polyethylene net or polypropylene tube were shown, but a product having good photocatalytic activity, adhesion and durability was obtained.
- Example 1-11 used alumina sol instead of silica sol, and a good product was obtained as in the case of silica sol.
- Example 17 shows the case where the thicknesses of the adhesive layer and the photocatalyst layer were 0.5 m and 0.1 m, respectively. However, the adhesion and the durability were good, and the photocatalytic activity was extremely thick. Despite being thin, it showed a high value.
- Example 1 The data of 19 to 23 are shown in Table 2.
- Example 1 A solution was prepared by adding polymethoxysiloxane (PS-2) to the resin solution used in 10 so that the Si02 content in the dry adhesive layer was 35% by weight. Solution.
- PS-2 polymethoxysiloxane
- An adhesive layer was applied to a soda lime glass substrate cut to 7 cm x 7 cm and having a thickness of 1 mm using a baker applicator, and a photocatalytic layer was applied using a bar coater.
- the drying temperature was the same as in the previous example.
- Example 19 was completely different from Example 19 except that the silica sol used in Example 19 was replaced by a 50:50 mixed sol solution of an aluminasol and a siliceous sol manufactured by Nissan Chemical Industries, Ltd.
- a photocatalyst carrier was prepared using the same raw materials and method.
- the obtained photocatalyst carrier had high adhesiveness and high catalytic activity.
- the total light transmittance of the obtained photocatalyst support was as high as 95%.
- Example—22 Application by Spray Method Using the adhesive layer solution and the photocatalyst layer solution used in Example-9, spray coating was performed on a soda lime glass substrate using a spray gun WIDER 88 manufactured by Iwata Coating Machine Industry Co., Ltd. Both the adhesive layer and the photocatalyst layer were dried at 120 ° C for 30 minutes.
- Example 12 A photocatalyst carrier was prepared by the same method with the same raw material, except that the xylene solution of the polyester resin was replaced with a 3% by weight of an epoxy resin methylethyl ketone solution in place of the polyester resin xylene solution. did.
- the obtained photocatalyst carrier had good adhesiveness and photocatalytic activity.
- the compositions and performance test results of the following Examples 24 to 35 are shown in Table 3.
- Example 35 the silica-alumina component was used as a sol that had been previously combined at this time.
- Ho 97 Example—24 to 125 used an acrylic silicone resin for the adhesive layer, and used fine particles of titanium oxide P-25 (C_1) manufactured by Japan Air Gill Co., Ltd. as the photocatalytic layer. It is obtained by preparing a raw material powder and a sol solution so as to have a composition containing 50% by weight, 25% by weight of a silica sol shown in (Z-1), and 25% by weight of an alumina sol shown in (Z-2). In the example using the composite, the adhesion after the boiling water test was good, and the durability and accelerated weather resistance were also good.
- Examples 12 to 13 use a resin containing polysiloxane for the adhesive layer.
- the photocatalyst layer contains fine particles of titanium oxide (C-11) in Examples 126 to 288.
- Example 1 The titania sol of (C-2) was used for 9-1 to 3-1 and the type and amount of the sol solution for forming the gel to be composited were changed, and the catalytic activity was good. Adhesion, durability, and accelerated weather resistance after the boiling water test were all good.
- the resin into which the polysiloxane has been introduced is either an acrylic-silicon resin (Examples 26, 27, 28, 28) or an epoxy-silicon resin (Examples 29, 30). Also, the adhesion, durability, and accelerated weather resistance after the boiling water test were good.
- a good resin was obtained by introducing the polysiloxane even with an acrylic resin (Example 31).
- Examples 13 and 13 show the results of supporting on a polyethylene net or polypropylene tube, but a product with good photocatalytic activity, adhesion and durability was obtained.
- Examples—32 to 135 used resin containing colloidal silicide for the adhesive layer, and had good catalytic activity, adhesion after boiling water test, durability, and accelerated weatherability. .
- KS-2 fine particle diameter
- the colloidal silica is introduced (Example-3). 4, 35)
- Example _ 29 the photocatalyst layer was prepared by adding nitric acid-containing titania sol (titanium oxide content: 12 wt. And catalyst chemical silicic sol (trade name: Cataloid SI-30)) to Nissan Chemical Aluminasol 200 was adjusted to pH 1.5 and dispersed, and a predetermined amount of surfactant was added to form a coating solution for the photocatalyst layer.
- the thickness of the adhesive layer and the photocatalyst layer was determined by dipping. The case of 0.5 m and 0.3 // m, respectively, was shown, but the adhesion and durability were good, and the photocatalytic activity showed a high value for the thin film thickness.
- Example 30 Even if the total content of the silica sol and the alumina sol in the photocatalytic layer was reduced to 30% by weight (Example 30), a good product was obtained.
- the photocatalytic activity of the sample subjected to the test was again examined by the amount of photodegradation of acetate aldehyde by the same method as in the initial stage, it was found that for all the samples, the amount of degradation of acetate aldehyde was exactly the same as the initial amount of acetate aldehyde. It showed decomposition activity and maintained the initial photocatalytic activity completely.
- the compositions and performance test results of the following Examples 36 to 53 are shown in Tables 4 and 5.
- the resin into which the polysiloxane has been introduced is an epoxy-silicon resin (Example 1, 43,
- Example 1 In the examples 4 4 to-47, the nitric acid titania sol (titanium oxide content: 12% by weight) was used for the photocatalyst layer in place of the fine particle titanium oxide (P-25) manufactured by Japan Air Gill Co., Ltd.
- a catalyst-based silicide sol (catalyst SI_30) and Nissan Chemical Aluminasol 200 or Nippon Soda's zirconazole are adjusted to PH 1.5 and dispersed, and a predetermined amount of interface
- Example 1 Even if the total content of acrylic silicone resin emulsion and silane coupling agent in the photocatalyst layer was reduced to 20% by weight (Example-47), a good product was obtained. However, when the content was reduced to 5% by weight (Comparative Example 18), even when the acrylic resin was added, the adhesion and durability were sharply reduced.
- Example 1 36 The samples obtained in 6--5 were subjected to a durability test using a black client under high temperature and high humidity, a boiling water immersion test, and an accelerated weathering test using a Sunshine Carbon Arc® user meter. The photocatalyst activity again by the same method as the initial one. Examination of the amount of photodegradation of acetate aldehyde revealed that all samples showed exactly the same value as the initial amount of degradation of acetoaldehyde, indicating that the initial photocatalytic activity was completely maintained. Was.
- Example 1 5 4 The samples obtained in 6--5 were subjected to a durability test using a black client under high temperature and
- a sample of the titanium oxide photocatalyst structure was prepared by the same method as that used in Example 42, and the antibacterial property was evaluated using the sample.
- the viability of E. coli was 92% after 1 hour, 91% after 2 hours, and 91% after 3 hours.
- the survival rate at 1 hour was 52%, 2 hours at 29%, and 3 hours at 11%.
- the viability of Escherichia coli was 76% after 1 hour, 54% after 2 hours, and 22% after 3 hours, even when irradiated with fluorescent light. It showed higher antibacterial properties than body samples.
- the following silicon compounds were used for the coating solution of the photocatalyst. (S-1) Tetraethoxysilane (Wako Pure Chemical Reagent Special Grade) 5% by weight ethanol solution
- the titanium oxide photocatalyst powder or sol solution in the sol solution shown in (Z-1) to (Z-3) and the silicon compound solution is adjusted to pH 1.5 depending on the raw materials used and types of additives. Adjusted to an appropriate range of ⁇ 9, the mixture was dispersed in water or a mixed solvent of water and ethanol as a solvent, and a predetermined amount of a surfactant was added to obtain a coating solution for forming a photocatalyst layer. The content of the components contained in the coating solution of the photocatalyst layer obtained, immediately after the preparation of the coating solution, and sealed. Table 6 summarizes the viscosity and the sedimentation state of the particles after the passage of days.
- Example 1 55 to 157 is an example of using titanium oxide powder (P-25) as the photocatalyst.
- the photocatalyst coating was applied 90 days after the addition of a trace amount of a silicon compound.
- the stability of the liquid is very good.
- Examples 158 to 160 used nitric acid-titania sol as the photocatalyst, and Examples 5.9 and -60 used silica sol and alumina sol as the composite metal oxide sol. It uses methyltriethoxysilane as the silicon compound.
- tetramethoxysilane as the silicon compound enabled the effect of maintaining the stability of the liquid to be obtained even with a small amount of addition.
- Example 63 powdery titanium oxide (P-25) and nitric acid titania sol were used in combination as a photocatalyst. Silicate sol and zirconium oxide were used as composite metal oxide sols. The stability of the coating solution and the sedimentation of the particles were improved by adding tetrasol and using the sol in combination.
- coating liquids were prepared by changing the type of silicon compound, and all of them were stable coating liquids with a predetermined addition amount.
- Comparative Examples 9 to 13 in which no silicon compound was added the viscosity of the coating solution was extremely increased after 90 days, and particles had to be sedimented after 90 days. When it was used as a coating solution, it was difficult to control the film forming conditions, and it was not possible to obtain a photocatalyst-coated product of constant quality.
- Example 1 The samples obtained in 67 to -71 were subjected to a durability test using black light under high temperature and high humidity, a boiling water immersion test, and an accelerated weathering test using a sunshine carbon arc weather meter. The photocatalytic activity was again examined by the amount of photodegradation of acetaldehyde by the same method as the initial one, and all samples showed exactly the same value as the initial amount of acetaldehyde decomposed. It turned out that it completely maintained.
- a sample of the titanium oxide photocatalyst structure was prepared by the same method as that used in Examples 67, and the antibacterial property was evaluated by the above method using the sample. As a result, the survival rate of E. coli in a dark place without light irradiation was 92% after 1 hour.
- the survival rate after 1 hour was 52% and that after 2 hours was 29%, compared to 91% after 2 hours and 91% after 3 hours. %, After 3 hours
- a polysiloxane [Methyl Silicate 51, manufactured by Colcoat Co., Ltd.] was added to a solution of xylene-isopropanol (50-50) containing 25% by weight of acrylo silicone resin with a silicon content of 3% by weight.
- the adhesive layer solution obtained by mixing 30% by weight of silicone resin and 5% by weight of curing agent (silane-capping agent) with acrylic resin is solid content of methyl ethyl ketone solvent. It was diluted to 10% by weight.
- This diluted solution was applied to a polyester film (Cosmoshine 50 m) A4100 manufactured by Toyobo Co., Ltd. with a microgravure coater (70 cm width) manufactured by Yasui Seiki Co., Ltd. // at a speed of 15 m / min, drying zone temperature 1 3
- a nitric acid-titania sol having a titanium oxide content of 20% by weight and a nitric acid-acid-titanium sol having a silicon oxide content of 20% were added to the polyester film having the adhesive layer formed thereon as a photocatalyst layer.
- This film can be used as an adhesive film to be applied to automotive window glass, window glass for general households, window glass of medical facilities, etc. It could also be used as a film to prevent shattering in case of damage.
- Xylene monoisopropanol 50/5) containing 25% by weight of acrylic silicone resin with a silicon content of 3% by weight in soda lime glass with a thickness of 1 mm cut into 5 cm x 5 cm. 0)
- a solution obtained by mixing 30% by weight of polysiloxane (Methyl Silicate 51, manufactured by Colcoat Co., Ltd.) with the acrylic resin is applied to the solution with an N0.7 bar coater, and the solution is coated with 100 °. C was dried for 60 minutes to form an adhesive layer.
- the photocatalyst layer is prepared by dispersing a nitric acid-titania sol containing 20% by weight of titanium oxide in a nitric acid-acidic silica sol containing 20% of silicon oxide in the presence of a surfactant.
- the coating solution for the layer was used. Using this solution, apply it to the surface of the above-mentioned adhesive layer also with a barco of N0.7 overnight, and dry it at 100 ° C for 60 minutes to obtain a photocatalyst-supporting glass.
- the adhesive layer solution used in Example 7 was diluted with a xylene-isopropanol (50/50) solution to a solid content of 25% by weight.
- the diluted solution was applied to a polyester film (Cosmo Shine) A4100 manufactured by Toyobo Co., Ltd. using a microgravure coater (70 cm width) manufactured by Yasui Seiki Co., Ltd. Gravure printing was performed at a speed of 10 m / min in a drying zone at a temperature of 130 ° C. Next, gravure printing was similarly performed on the polyester film having the adhesive layer formed thereon using the coating solution for the photocatalyst layer used in Example 77 to obtain a photocatalyst layer having a dry film thickness of 3 //. The formed polyester film was obtained. (S amp l e. 5)
- Polysiloxane (Methyl Silicate 51, manufactured by Colcoat Co., Ltd.) was added to the acrylic silicon resin in a xylene solution containing 20% by weight of an acrylic silicone resin with a silicon content of 20% by weight. 30% by weight, and immersed in a solution diluted to a solid content of 20% by weight with an isopropanol solution, and immersed in Toray's VDT filter-E-fiterter III. And dried at 100 ° C. for 20 minutes to form an adhesive layer. Next, the VDT protective filter having the adhesive layer formed thereon was used in Example 77.
- Example 77 The adhesive layer solution used in Example 7 was diluted using a xylene-isopropanol (50/50) solution to a solid content of 20% by weight. The diluted solution was spray-coated on a case of a Hitachi Ltd. HIT-1 type telephone using a spray gun WIDER 88 type manufactured by Iwata Coating Machine Industry Co., Ltd. After drying at 100 for 20 minutes, the solution of the photocatalytic layer used in Example 1 was diluted with ion-exchanged water to a solid content of 8% by weight, and sprayed in the same manner. did. After drying at 100 ° C. for 2.0 minutes, a telephone case carrying a photocatalyst was obtained. (S ample. 7).: Example 81 1 Eyeglass Lens
- a solution prepared by mixing 1) with 20% by weight of the acrylic silicone resin an adhesive layer was formed by the same immersion method as in Example 9 and then at 100 ° C for 20 minutes. Dried. After cooling at room temperature, a nitric acid titania sol with a titanium oxide content of 15% was dispersed in a nitric acid silica sol with a silicon oxide content of 15% as a photocatalyst layer in the presence of a surfactant, and the photocatalyst layer was applied. The solution was used. Using this solution, a photocatalytic layer is applied to the surface of the adhesive layer by the same dipping method,
- Example 8 2 Curtain Cut out 7cm x 7cm of curtain cloth hospia (for schools and hospitals) manufactured by Kawashima Textile Co., Ltd. and 15% by weight xylene isopropanol with 3% by weight silicone content epoxy resin. (50/50) solution is impregnated with a solution obtained by mixing 20% by weight of polysiloxane (methyl silicate 51, manufactured by Corcolt Co., Ltd.) with the acrylic silicone resin. Dry at 120 ° C. for 120 minutes.
- polysiloxane methyl silicate 51, manufactured by Corcolt Co., Ltd.
- Example 83 Non-woven fabric. A non-bleached product (weight per unit weight: 50 g / m 2 ) of Kotton non-woven fabric (trade name: Olkos) manufactured by Seibo Co., Ltd.
- Example 86 Aluminum sash
- polysiloxane methylsilicate 51, manufactured by Colcoat Co., Ltd.
- a nitric acid-titania sol having a titanium oxide content of 20% by weight was dispersed as a photocatalyst layer in a nitric acid-acidic sol having a silicon oxide content of 20% in the presence of a surfactant to form a photocatalytic layer.
- the coating solution was used. This solution was applied to the surface of the adhesive layer with a bar coater of N0.7 in the same manner, and dried at 130 ° C for 10 minutes to obtain an aluminum plate supporting a photocatalyst. (Sam ⁇ 1e.13)
- Example 8 7 Stainless steel plate
- Example 86 The adhesive layer solution used in 6 was diluted with a xylene-isopropanol (50/50) solution to a solid content of 5% by weight. A sample obtained by cutting a SUS316 stainless steel plate (0.2 mm thick) into 7 cm x 7 cm is immersed in this diluted solution, pulled up, allowed to stand, and dried at 120 ° C for 20 minutes. An adhesive layer was formed on the surface of the stainless steel plate. Next, the stainless steel plate on which the adhesive layer was formed was immersed in a solution prepared by diluting the coating solution for the photocatalyst layer used in Example 86 to 10% by weight with ion-exchanged water, and pulled up. After drying at 20 ° C for 20 minutes, a stainless steel plate supporting the photocatalyst was obtained. (S ample. 14) Example 8 Printed plate
- Polysiloxane (Methyl Silicate 51, manufactured by Colcoat Co., Ltd.) was added to an acrylic solution containing 20% by weight of an acrylic silicone resin containing 20% by weight of the acrylic silicone resin. 30% by weight, and immerse a 0.1 mm thick tin plate cut into 7 cm x 7 cm into a solution diluted to 20% by weight as a solid with isopropanol solution. Then, it was pulled up and dried at 100 ° C. for 60 minutes to form an adhesive layer. Next, the tin plate on which the adhesive layer was formed was immersed in a solution obtained by diluting the coating solution for the photocatalyst layer used in Example 86 to 10% by weight with ion-exchanged water, and pulled up. For 60 minutes to obtain a tin plate supporting a photocatalyst. (Sammple.15)
- Acrylic silicone resin with a silicon content of 3% by weight was added to Neowood (2.5 mm thick) printed plywood cut to 7 cm x 7 cm by Eidai Sangyo Co., Ltd.
- Weight% included A solution obtained by mixing a xylene-isopropanol (50/50) solution with a polysiloxane (methyl silicate 51, manufactured by Colcoat Co., Ltd.) in an amount of 30% by weight with respect to the acrylic-silicon resin was mixed with N 0.
- the resultant was applied with a bar coater of 0.7 and dried at 100 ° C. for 30 minutes to form an adhesive layer.
- the adhesive layer solution used in Example 90 was diluted with a xylene-isopropanol (5.0.50) solution to a solid content of 5% by weight.
- Sessui Chemical Co., Ltd.'s Ethrone Neo-Lamper-FFU-50 was cut into 7 cm x 7 cm x 7 cm, immersed in wood, pulled up and allowed to stand at 100 ° C. After drying for 0 minutes, an adhesive layer was formed on the surface of the synthetic wood.
- the synthetic wood on which the adhesive layer was formed was immersed in a solution obtained by diluting the coating solution for the photocatalyst layer used in Example 90 to 10% by weight with ion-exchanged water and pulled up. It was dried for 120 minutes with C to obtain a photocatalyst-supporting synthetic wood.
- Polysiloxane Metal Silicate 51, manufactured by Colcoat Co., Ltd.
- An adhesive layer was formed by the same dipping method as in Example 91 using a solution prepared by mixing 20% by weight with respect to the crystalline silicon resin, and dried at 100 ° C. for 20 minutes. .
- nitric acid titania sol containing 5% titanium oxide was used as a photocatalyst layer. It was dispersed in a nitric acid-based silicic acid sol having a nitrogen content of 5% in the presence of a surfactant to obtain a coating solution for the photocatalytic layer. Using this solution, a photocatalyst layer was applied to the surface of the adhesive layer by the same dipping method, and dried at 100 ° C. for 20 minutes to obtain a photocatalyst-coated wooden door material. (S amp l e. 1 9)
- the photocatalyst-supporting structure of the present invention has a high photocatalytic activity, and is a glass, a plastic, a metal material, a cloth, a wood, and a wood-based material that supports a photocatalyst that is not easily deteriorated and has high durability.
- a high photocatalytic activity is a glass, a plastic, a metal material, a cloth, a wood, and a wood-based material that supports a photocatalyst that is not easily deteriorated and has high durability.
- products in a wide range of application fields such as lenses, various window glasses, adhesive films, decorative sheets, wallpaper, curtains, blinds, and other building materials such as interior products for antibacterial, deodorizing, and antifouling purposes. can do.
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Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE69637493T DE69637493T2 (de) | 1995-06-19 | 1996-06-18 | Trägerstruktur mit photokatalysator und photokatalytisches beschichtungsmaterial |
KR1019970709547A KR100280910B1 (ko) | 1995-06-19 | 1996-06-18 | 광촉매 담지 구조체 및 광촉매 코팅제 |
EP19960917713 EP0923988B1 (en) | 1995-06-19 | 1996-06-18 | Photocatalyst-carrying structure and photocatalyst coating material |
US08/981,303 US6228480B1 (en) | 1995-06-19 | 1996-06-18 | Photocatalyst-carrying structure and photocatalyst coating material |
JP9502929A JP3038599B2 (ja) | 1995-06-19 | 1996-06-18 | 光触媒担持構造体および光触媒コーティング剤 |
Applications Claiming Priority (22)
Application Number | Priority Date | Filing Date | Title |
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JP7/175422 | 1995-06-19 | ||
JP17542295 | 1995-06-19 | ||
JP7/349334 | 1995-12-20 | ||
JP7/349338 | 1995-12-20 | ||
JP34933795 | 1995-12-20 | ||
JP34933495 | 1995-12-20 | ||
JP34933695 | 1995-12-20 | ||
JP7/349335 | 1995-12-20 | ||
JP7/349336 | 1995-12-20 | ||
JP34933895 | 1995-12-20 | ||
JP34933595 | 1995-12-20 | ||
JP7/349337 | 1995-12-20 | ||
JP35374295 | 1995-12-28 | ||
JP7/353742 | 1995-12-28 | ||
JP8/34350 | 1996-01-29 | ||
JP3435096 | 1996-01-29 | ||
JP8/52469 | 1996-02-15 | ||
JP5246996 | 1996-02-15 | ||
JP6367396 | 1996-02-26 | ||
JP8/63673 | 1996-02-26 | ||
JP8/150115 | 1996-05-21 | ||
JP8150115A JPH09310039A (ja) | 1996-05-21 | 1996-05-21 | 光触媒コーティング剤 |
Publications (2)
Publication Number | Publication Date |
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WO1997000134A1 true WO1997000134A1 (en) | 1997-01-03 |
WO1997000134A8 WO1997000134A8 (en) | 1999-04-01 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP1996/001669 WO1997000134A1 (en) | 1995-06-19 | 1996-06-18 | Photocatalyst-carrying structure and photocatalyst coating material |
Country Status (5)
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US (1) | US6228480B1 (ja) |
EP (2) | EP0923988B1 (ja) |
CN (1) | CN1081490C (ja) |
AT (1) | ATE391553T1 (ja) |
WO (1) | WO1997000134A1 (ja) |
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Also Published As
Publication number | Publication date |
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WO1997000134A8 (en) | 1999-04-01 |
CN1081490C (zh) | 2002-03-27 |
CN1188428A (zh) | 1998-07-22 |
EP1955768A1 (en) | 2008-08-13 |
EP0923988A4 (ja) | 1999-07-14 |
EP0923988A1 (en) | 1999-06-23 |
EP0923988B1 (en) | 2008-04-09 |
US6228480B1 (en) | 2001-05-08 |
ATE391553T1 (de) | 2008-04-15 |
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