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WO2002085989A1 - Materiau de revetement photocatalytique presentant une activite photocatalytique et des proprietes d'adsorption, et procede de preparation associe - Google Patents

Materiau de revetement photocatalytique presentant une activite photocatalytique et des proprietes d'adsorption, et procede de preparation associe Download PDF

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Publication number
WO2002085989A1
WO2002085989A1 PCT/KR2002/000769 KR0200769W WO02085989A1 WO 2002085989 A1 WO2002085989 A1 WO 2002085989A1 KR 0200769 W KR0200769 W KR 0200769W WO 02085989 A1 WO02085989 A1 WO 02085989A1
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weight
sol composition
photocatalytic coating
photocatalytic
coating sol
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Ceased
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English (en)
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Tai-Kyu Lee
Young-Jin Yoon
Woo-Sug Yoon
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NANOPAC Ltd
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NANOPAC Ltd
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Priority to US10/475,514 priority Critical patent/US20050126428A1/en
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Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances

Definitions

  • the present invention relates to a photocatalytic coating sol composition and a method for preparing the same, and more particularly to an application to an environmental purifying system in a manner of coating a photocatalytic coating sol composition, having high adsorption property as well as high photocatalytic activity, on meshes of metal such as stainless steel, non-ferrous metal such as aluminum, non-woven fabric, ceramic filter and plastics such as polyethylene (PE) filter, by means of an inorganic binder, by using common coating techniques such as spraying method or dipping method etc. at room temperature.
  • metal such as stainless steel, non-ferrous metal such as aluminum, non-woven fabric, ceramic filter and plastics such as polyethylene (PE) filter
  • PE polyethylene
  • the conventional method for treating environmental contaminants could be classified into two methods.
  • One is a physico-chemical method which includes adsorption, cooling condensation, solvent scrubber, catalytic oxidation method.
  • another is a biological treatment method.
  • the solvent scrubber method is a type of a chemical deodorization method in which the contaminants are neutralized due to chemicals, whereby removal rate of the contaminants is high for limited areas.
  • a method for biological treating the contaminants using microorganisms has been widely used in recent years owing to low initial investment costs as well as operating costs, has been studied actively in industrially advanced countries such as Europe and North America, and thus has reached to a commercialization step.
  • various microorganisms capable of removing the contaminants are immobilized in a carrier, which is advantageous in removing the contaminants in a high rate. And also, it allows using small-sized equipments.
  • the method has technical problems, for example, contaminants used as nutrients for growth of the microorganisms must be continuously administered into a reactor where a substantial contaminants removal is performed, the carrier must be washed periodically, the microorganisms must be well controlled, and process of this method must be operated continuously.
  • Korean Patent Application No. 1999-0052838 discloses a filter using photocatalyst coated with titanium dioxide (Ti0 2 ), zinc oxide (ZnO) and silver (Ag) etc. on filter such as non-woven fabric, activated carbon and Zeolite etc.
  • Korean Patent Application No. 2000-0034908 discloses a method for treating volatile organic compounds by using photocatalyst
  • Korean Utility Model Application No. 2000-0029990 discloses a device for treating water by using titanium oxides.
  • the photocatalytic oxidation refers to the decomposing reaction of gaseous or liquid phase organic materials which are adsorbed on the surface of the photocatalyst owing to the strong oxidation of hydroxyl radicals (-OH) generated by a hole, wherein the hole is generated together with an electron when a light energy, more than the bandgap energy, is irradiated on the photocatalyst.
  • -OH hydroxyl radicals
  • the photocatalyst shows catalytic activity by absorbing light energy, and the generated oxidation strength is used to decompose environmental contaminants by oxidation.
  • Representative materials inducing photocatalytic reaction may be, for example, Ti0 , Zn0 2 , ZnO, SrTi0 3 , CdS, GaP, InP, GaAs, BaTi0 3 , KNb0 3 , Fe 2 0 3 , Ta 2 0 5 , W0 3 , Sn0 2 , Bi 2 0 3 , NiO, Cu 2 0, SiO, Si0 2 , MoS 2 , InPb, Ru ⁇ 2 , Ce0 2 etc., and could be used by adding metals such like Pt, Rh, Ag, Cu, Sn, Ni, Fe etc. and metal oxide thereof to the above photocatalyst.
  • titanium dioxide (Ti0 2 ) is mostly used because it is harmless to human body, exhibits excellent photocatalytic activity, good photo-corrosion resistance and
  • the titanium dioxide absorbs and reacts at a wavelength less than 388nm and generates the electron (conduction band) and the hole (valence band).
  • glow lamp and mercuric lamp besides solar energy lamp could be used for UV ray as a light source.
  • the electron and the hole generated by the above reaction recombine with each other within 10 "12 sec to 10 "9 sec.
  • the contaminants are adsorbed on the surface prior to recombination of the electron and the hole, the contaminants are decomposed by the electron and the hole.
  • reaction mechanism of this photocatalyst can be represented as the following reaction formulas 1 to 5. [Reaction formula 1]
  • the technique has been practically used in anti-fouling field, such as a filter for an air cleaner, the filter deodorizing odor components (e.g. cigarette smoke) by using titanium dioxide as photocatalyst, antibiotic filter having antibacterial function in water or atmosphere, glass and tile. And, a filter being coated with a photocatalyst can be applied. to photocatalytic system to decompose the volatile organic compounds.
  • the photocatalytic reaction is a surface reaction, there is a need for developing a technique capable of adsorbing a large amount of organic contaminants or odor materials.
  • a method for coating photocatalyst via a liquid phase which is most commonly used, uses titanium alkoxide as a starting material to prepare a sol composition, which coats a carrier (Japanese patent publication No. 5-253544).
  • the method requires complex process steps such as generating photocatalytic particles on the carrier after coating, crystallization of anatase type having high photocatalytic activity, and sintering at the temperature range of 400 to 600 °C to give adherence to a carrier, resulting in high manufacturing cost.
  • photocatalytic coating method via a gaseous phase not using photocatalytic coating sol composition includes spattering method or chemical vapor depositing method disclosed in Japanese Patent publication No. 60-44053.
  • problems such as high initial investment cost due to the manufacturing of equipments, high consumption of electric power and manufacturing time due to the increase of coating film thickness.
  • titanium dioxide is formed as a thin-film on a support according to the sol-gel method, it requires much time for decomposing contaminants because of limited contact area of contaminants on the thm-film containing photocatalyst.
  • filter for air handling unit such as air purifier, air-conditioner etc. which is used for removing odor material and the like, requires about 10 "3 sec of treatment time, and thus it requires development to the sol for coating having high adsorption power and high photocatalytic activity.
  • sol composition in order to uniformly disperse different kinds of particles between different kinds of particles in solution state, different kinds of sol composition were physically mixed with each other (U.S. patent No. 5,591,380), or two kinds of alkoxides as starting materials were dissolved simultaneously into the solvent to prepare sol composition (U.S. patent No. 4,176,089).
  • the stability of sol composition decreases and turns into gel in short time.
  • the coating film becomes thick and is delaminated from the carrier after the heating treatment.
  • the methods have the disadvantage in that the condition of the manufacture process must be controlled accurately when sol particles are dispersed by dissolving start materials simultaneously.
  • the present inventors have made a research to develop a photocatalytic coating composition having high adsorption and high photocatalytic activity, and as a result, the present invention has been completed on the basis of the discovery described below.
  • An object of the present invention is to provide a photocatalytic coating sol composition and method for preparing the same, capable of preventing de- lamination of secondary contaminants generated by transient photocatalytic reaction and having high photocatalytic activity.
  • Another object of the present invention is to provide a method capable of decomposing and removing environmental contaminants and harmful microorganisms etc. by coating filters with the photocatalytic coating sol composition for water treatment and air treatment coated according to a method such as spray method or dipping method.
  • a photocatalytic coating sol composition comprising 0.1 % to 20% by weight of a photocatalyst, 0.1% to 10 % by weight of an inorganic adsorbent, 1 % to 20 % by weight of an inorganic binder and 55 % to 95 % by weight of an organic solvent.
  • a photocatalytic coating sol composition comprising 0.1 % to 20 % by weight of a photocatalyst, 0.1 % to 10 % by weight of an inorganic adsorbent, 1 % to 20 % by weight of an inorganic binder, 55 % to 95 % by weight of an organic solvent and 0.1 % to 10 % by weight of a metal compound.
  • a method for preparing the photocatalytic coating sol composition comprising the steps of mixing 1 % to 20 % by weight of an inorganic binder, 55 % to 95 % by weight of an organic solvent and if necessary, 0.1 % to 0.5 % by weight of a strong acid or a strong base and then stirring at 1000 to 1500 rpm for 10 to 30 min at room temperature, adding 0.1 % to 20% by weight of a photocatalyst powder and 0.1% to 10 % by weight of an inorganic adsorbent into the mixture and then treating for 10 to 50 min in an ultrasonic device, and if necessary, adding 0.1% to 10% by weight of a metal compound into the mixture.
  • the photocatalyst may be used either alone or mixture of at least two kinds of photocatalytic metal oxides selected from Ti0 2 , Zn0 2 , ZnO, CaTiO, W0 3 , Sn ⁇ 2, M0O3, Fe 2 0 3 , InP, GaAs, BaTi0 3 , Knb0 3 , Fe 2 0 3 and Ta 2 0 5 , preferably Ti0 2 and/or ZnO.
  • a small sized photocatalyst particle shows more excellent photocatalytic property. Therefore, the average diameter of particle should be from 1 to 50nm, and preferably 1 to lOnm.
  • the reaction rate of the photocatalyst is increased by adding 0.01% to 5% by weight of a metal or a metal oxide, for example, palladium, platinum, radium, tungsten, gold, silver and copper etc. of the total weight of the photocatalyst.
  • a metal or a metal oxide for example, palladium, platinum, radium, tungsten, gold, silver and copper etc.
  • the durability of the photocatalyst can be improved by combining the photocatalyst with hindered amine type photo-stabilizer and triazole- based UV adsorbent to inhibit deterioration of photocatalytic coating film due to photocatalytic reaction.
  • the inorganic adsorbent in accordance with the present invention is not particularly limited, but preferably high adsorbent inorganic material which is capable of adsorbing odor material and harmful materials during photocatalytic reaction, and more preferably, for example, magnesium or calcium-containing silicates, talc, diatomite, zeolite coated with silver or copper ion.
  • the inorganic binder in accordance with the present invention may be used, for example, isopropoxide compound, silane compound etc., preferably isopropoxide compound such as titanium isopropoxide.
  • acid or base catalyst may be added in small amounts.
  • the organic solvent used in the present invention may be alcohol having lower alkyl group, preferably anhydride ethanol or isopropanol etc.
  • the metal compound in the present invention is not particularly limited, but preferably the materials capable of improving antibiotic function and color of the materials may preferably be used either alone or as a mixture of more than two species selected from a copper compound such as acetylacetonate (copper (II)), copper acetate monohydrate (copper (II)) etc., a silver compound such as silver acetate etc., bengala, vermilion, cadmium red, yellow earth, cadmium yellow, emerald rock, chromium oxide green, Prussian blue, cobalt blue, manganese or carbon black, and more preferably a copper compound.
  • a copper compound such as acetylacetonate (copper (II)), copper acetate monohydrate (copper (II)) etc.
  • a silver compound such as silver acetate etc., bengala, vermilion, cadmium red, yellow earth, cadmium yellow, emerald rock, chromium oxide green
  • an inorganic adsorbent is added and treated for 10 to 50 min in an ultrasonic device to obtain the coating sol composition according to the present invention.
  • the inorganic adsorbent is adsorbed on the coating film while harmful materials such as odor materials, primarily decomposable materials are decomposed by the photocatalyst, secondary contaminants are adsorbed on the coating film after photocatalyzing primarily decomposable materials and thus the harmful materials will be less emitted into the atmosphere by photo-decomposition of the photocatalyst.
  • a metal compound may be used to enhance antibiotic function of the photocatalytic coating sol composition according to the present invention or to enhance color development of the coating film by irradiating ultraviolet light on the coating film.
  • the photocatalytic coating sol composition according to the present invention may be uniformly dispersed with different kinds of oxides onto the coating film, the method can be more easily and commercially used than the prior methods. Also, in order to control hydrolysis rate of inorganic binder, small amounts of acid or base catalyst may be added.
  • the photocatalytic coating sol composition according to the present invention may be coated on the desired substrate according to a printing method, a spraying method, a dipping method etc. and dried, and preferably the spraying method or the dipping method may be used.
  • the drying temperature in the spraying and dipping method depends on solvents, it is generally 50 to 200 °C, preferably 100 to 150 °C.
  • the substrate is not particularly limited, but any material capable of being coated with the photocatalytic coating sol composition prepared according to the present invention is preferred.
  • the substrates include various carriers which require effects of antibiotic, deodorization, pollution control etc., or filters for water treatment and air pollution preventing equipment, metal, alloy, glass, curtain, wall paper, package, plastics and papers.
  • the thickness of the coating film For coating the photocatalytic coating sol composition on the substrate, the thickness of the coating film must be controlled according to use. If the thickness of the coating film is larger than 0.1 ⁇ m, the photocatalytic layer is firmly adherent on the substrate and thus the coating structure having high durability is obtained, and furthermore as the thickness of the coating film increases, the photocatalytic activity increases too.
  • the photocatalytic activity does not increase accordingly because the light source can not be sufficiently transmitted into the bottom of the photocatalyst layer. Because the photocatalytic activity is high if the thickness is less than the size of 5 ⁇ m, it is preferable that the photocatalytic coating film is selected taking into account of the light transmission properties.
  • the thickness of the coating film in the range of 20 to 50 ⁇ m to enhance adsorbent property of the contaminants. Therefore, the thickness of the photocatalytic layer can be determined in the range of 5 to 50 ⁇ m.
  • the photocatalytic coating sol composition in accordance with the present invention can be applied to various carriers which require an effect of antibiotic, deodorization, pollution control, for example interior goods such as curtain, wall paper, commodities such as tent, umbrella, scarf etc., packaging vessel such as food package etc., agricultural field such as raising seedling sheet etc,.
  • the metal including photocatalytic function may be used as substrate with single metal of uminum, iron, copper etc. and further all kinds of alloy such as stainless, pearl, brass, aluminum alloy, titanium alloy etc.
  • the coating film consisting of the photocatalytic coating sol composition according to the present invention can be formed onto the metal sheet or plate coating with common paint and colored copperplate according to the shape or quality of the used metal. If the adherent layer and the coating film of the photocatalyst have high photo-transmission rate and transparency, its applicability can be improved because the color tone of basic paint is not damaged.
  • Photocatalyst substrate structure according to the present invention makes it possible to function simultaneously such as decomposition, antibiotic and deodorization of harmful materials by applying to window glass of automobile or all kinds of conveyance, window glass of architecture, filter for refrigeration • chilling showcase or environmental purifying system by utilizing the functions and enhance pollution prevention function of glass surface,
  • plastic filters e.g. polyethylene filter, polypropylene filter etc.
  • FIG. 1 shows a graph of photocatalytic activity of metal mesh coated with a photocatalytic coating sol composition prepared without adding inorganic adsorption and metal compound;
  • FIG. 2 shows a graph of photocatalytic activity of metal mesh coated with a photocatalytic coating sol composition according to Example 6 of the present invention
  • FIG. 3 shows a graph of photocatalytic activity of metal mesh coated with a photocatalytic coating sol composition according to Example 7 of the present invention
  • FIG. 4 shows a graph of antibiotic experiment results of metal mesh coated with a photocatalytic coating sol composition prepared according to the present invention and photocatalytic coating sol composition prepared without adding inorganic adsorbent and metal ions, respectively;
  • FIG. 5 shows a graph of de-colorization experiment result of polyethylene filter coated with a photocatalytic coating sol composition prepared according to the present invention
  • FIG. 6 shows a graph of activity experiment result of polyethylene filter coated with a photocatalytic coating sol composition prepared according to the present invention
  • FIG. 7 shows the graph of saturated activity experiment result of polyethylene filter coated with a photocatalytic coating sol composition prepared according to the present invention
  • FIG. 8 shows an electron microscope photograph taken from the surface of polyethylene filter coated with a photocatalytic coating sol composition prepared according to the present invention.
  • FIG. 9 shows an electron microscope photograph taken from section of polyethylene filter coated with a photocatalytic coating sol composition prepared according to the present invention.
  • Example 2 5% by weight of titanium isopropoxide [Junsei Chemical Co., Ltd.], 78.5% by weight of anhydrous ethanol and 0.2% by weight of hydrochloric acid were mixed and then stirred with 1200rpm for 20 min at room temperature. Next, 10% by weight of titanium dioxide powder [Degussa P25, German] was added into the mixture. In the mixed solution, 6% by weight of talc [DUKSAN PURE CHEMICAL
  • Example 2 The same process as in Example 1 was carried out, except that, instead of 6% by weight of talc, 5% by weight of diatomite [DUKSAN PURE CHEMICAL Co., Ltd.] was used.
  • Example 2 The same process as in Example 2 was carried out, except that, instead of 0.3% by weight of copper acetate hydrate, 0.3% by weight of hydrate silver acetate [Junsei Chem. Co., Ltd. Japan] was used.
  • the sol composition for coating prepared according to Example 1 was coated on a metal mesh [Al salongs 4x8mm, 0.4T, Hyungjei Metalas Co., Korea] according to the spraying method (diameter: 1.5, pressure: 4KG) at room temperature and then dried at the temperature of 120 to 150 °C, to obtain metal mesh coated with photocatalyst.
  • Example 6 The same process as in Example 6 was carried out, except that, instead of the sol composition for coating prepared by Example 1, the sol composition for coating prepared by Example 2 was used.
  • Example 6 The same process as in Example 6 was carried out, except that, instead of the sol composition for coating prepared by Example 1, the sol composition for coating prepared by Example 3 was used.
  • Example 10 The same process as in Example 6 was carried out, except that, instead of the sol composition for coating prepared by Example 1, the sol composition for coating prepared by Example 4 was used. ⁇ Example 10>
  • the sol composition for coating prepared according to Example 5 was coated on a polyethylene filter [SW80M, Shinwu Co., Korea] according to the spraying method (diameter: 1.5, pressure: 4KG) at room temperature and then dried at a temperature of 60 °C, to obtain polyethylene filter coated with the photocatalyst.
  • trichloroethylene C 2 HC1 3 , TCE
  • Initial concentration of the trichloroethylene was about 2000ppm
  • volume of reactor was 125cm 3
  • the metal mesh was irradiated by black light lamp (wavelength 300nm to 368nm, maximum wavelength 400nm)[4W BLB, Sankyo denki, Japan]
  • decomposition rate of the trichloroethylene was measured with FTIR spectrometer [Perkin Elmer, Spectrum one FT-IR spectrometer].
  • FIG.1 shows the activity of metal mesh coated with photocatalytic coating sol composition prepared without adding inorganic adsorbent and metal compound according to the Comparative Example
  • FIG. 2 shows the activity of metal mesh coated with photocatalytic coating sol composition prepared according to Example 6 of the present invention
  • FIG. 3 shows the activity of metal mesh coated with photocatalytic coating sol composition prepared according to Example 7 of the present invention.
  • photocatalytic coating sol composition being prepared without adding inorganic adsorbent and metal compound on photocatalyst filter for air-conditioner and air-purifier.
  • Example That means that the secondary contaminants was not emitted into the atmosphere because it was adsorbed by adding high adsorptive inorganic.
  • Japan] of 0.8ppm was added into the petri dish (diameter: 100mm, height: 15mm), and the polyethylene filter coated with photocatalyst prepared according to Example 10 was dipped in the petri dish, and then, de-colorization degree of aqueous solution was observed by irradiation with black light lamp[4W BLB, Sankyo Denki, Japan] of wavelength of 300 to 368nm, maximum wavelength of 400nm, and 4W equipped at a distance of 13 cm from the petri dish.
  • black light lamp[4W BLB, Sankyo Denki, Japan] of wavelength of 300 to 368nm, maximum wavelength of 400nm, and 4W equipped at a distance of 13 cm from the petri dish black light lamp[4W BLB, Sankyo Denki, Japan] of wavelength of 300 to 368nm, maximum wavelength of 400nm, and 4W equipped at a distance of 13 cm from the petri dish.
  • the polyethylene filter coated with photocatalyst prepared by Example 10 was placed in the center of closed SUS reactor having a volume of 125L and then trimethylamine (TMA) as odor material was poured into the reactor at a rate of 0.83m/s. After pouring the trimethylamine
  • TAM removal rate depending on time was measured, as shown in FIG. 6.
  • removal rate of the trimethylamine was 82.2% after 10 min and 90.41% after 30min, respectively.
  • the experiment was set as 1 cycle and after completing the 1 cycle, light was irradiated for 1 hour with black light lamp [4W BLB, Sankyo Denki, Japan] on the polyethylene filer coated with the photocatalyst, and followed by repeating the same process as described above.
  • the second experiment was set as 2 cycle and the cycles was repeated.
  • Antibiotic test Antibiotic property of polyethylene filter coated with photocatalytic coating sol composition prepared according to Example 10 by using Shake Flask Method was measured.
  • Shake Flask Method can be performed as follows:
  • Bacteria Decreasing Rate [(bacteria of blank after 24hours - bacteria number of coated goods after 24 hours)/bacteria number of blank after 24hours] x 100
  • the blank was the original sample without coating, for example polyethylene filter without the photocatalytic coating sol composition coating.
  • the known bacteria strains used in the Shake Flask method were Staphylococcus aureus ATCC 6538 and Escherichia coli ATCC 25992. The result is shown in following Table 1. As shown in the Table 1, microorganisms increasing rate in Examples 7 and 10 using polyethylene filter coated with photocatalytic coating sol composition was very low, while bacteria was increased by 30% to 40% in the blank sample.
  • Antimicrobial property for polyethylene filter coated with photocatalytic coating sol composition prepared according to the Example 10 was tested by using ASTM G-21 as test standard.
  • the 0 grade refers to no growth of the known strain.
  • the present invention uses an inorganic adsorbent, and includes effective techniques used in environmental contaminants treatment system or air conditioning plant such as air-conditioner and air-cleaner.

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Abstract

L'invention concerne une composition de sol de revêtement photocatalytique et un procédé de préparation associé. Cette composition de sol de revêtement photocatalytique contient de 0,1 % à 20 % en poids d'un photocatalyseur, de 0,1 % à 10 % en poids d'un adsorbant inorganique, de 1 % à 20 % en poids d'un liant inorganique, de 55 % à 95 % en poids d'un solvant organique et, si nécessaire, de 0,1 % à 10 % en poids d'un composé métallique. L'invention permet, en particulier, d'éliminer des substances nocives par le revêtement d'une composition de sol de revêtement photocatalytique préparée à partir d'un photocatalyseur, d'un adsorbant inorganique, d'un liant inorganique, d'un composé métallique et d'un solvant organique sur un filtre métallique, tel que de l'aluminium etc., et un filtre plastique, tel que du polyéthylène et du polypropylène etc., cette composition étant utilisée dans un système de traitement de polluants ou dans une installation de conditionnement d'air, telle qu'un conditionneur d'air et un filtre à air, selon n'importe quelle technique de revêtement ordinaire, telle qu'un procédé de pulvérisation ou un procédé d'application au trempé etc., à température ambiante.
PCT/KR2002/000769 2001-04-25 2002-04-25 Materiau de revetement photocatalytique presentant une activite photocatalytique et des proprietes d'adsorption, et procede de preparation associe Ceased WO2002085989A1 (fr)

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KR20010022270 2001-04-25
KR2001/0022270 2001-04-25

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