KR100447818B1 - Method for Preparing a Photocatalyst Activated by Visible Light - Google Patents

Method for Preparing a Photocatalyst Activated by Visible Light Download PDF

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KR100447818B1
KR100447818B1 KR1020030097633A KR20030097633A KR100447818B1 KR 100447818 B1 KR100447818 B1 KR 100447818B1 KR 1020030097633 A KR1020030097633 A KR 1020030097633A KR 20030097633 A KR20030097633 A KR 20030097633A KR 100447818 B1 KR100447818 B1 KR 100447818B1
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photocatalyst
organic solvent
visible light
visible
sol
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KR1020030097633A
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Korean (ko)
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김영규
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엔비넷 주식회사
김영규
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    • 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
    • B01J37/03—Precipitation; Co-precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

PURPOSE: To provide a visible ray activated photocatalyst sol having characteristics of sterilizing air inside a room in which fluorescent lamps or electric heating lamps are used with sunlight and microorganisms of building materials such as wallpaper and cabinets and decomposing thus eliminating formaldehyde and volatile organic compounds, and a method for preparing the same. CONSTITUTION: The method comprises a step (a) of dissolving titanium isopropoxide (Ti(OCH(CH3)2)4) that is a photocatalyst into an organic solvent; a step (b) of obtaining a TiO2 photocatalyst sol by reacting reactants as adding string acid to the mixed solution after adding distilled water to the photocatalyst dissolved organic solvent; and a step (c) of obtaining a photocatalyst sol activated by visible rays by coprecipitating the mixture with the TiO2 photocatalyst sol after preparing a mixture by mixing a solution prepared by dissolving AgO, CuO or a metal mixture thereof into an acid with a solution prepared by mixing binder with organic solvent in a mixing ratio of 1:1 to 1:5.

Description

가시광선 광촉매의 제조방법 {Method for Preparing a Photocatalyst Activated by Visible Light}Method for preparing visible photocatalyst {Method for Preparing a Photocatalyst Activated by Visible Light}

본 발명은 형광등이나 전열등의 가시광선에서 공기나 건축관련 자재의 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 가시광선 광촉매 및 그 제조방법에 관한 것으로, 보다 구체적으로는, 광촉매제인 TiO2졸을 ZnO, AgO, CuO등의 금속혼합물 및 바인더가 혼합된 금속용액과 공침하는 것을 특징으로 하는 가시광선에 의해 활성화되는 광촉매의 제조방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a visible light photocatalyst for sterilizing microorganisms of air or construction-related materials or removing formaldehyde and volatile organic substances (VOC) from visible light such as fluorescent lamps and heat transfer lamps, and more particularly, a photocatalyst. The present invention relates to a method for preparing a photocatalyst activated by visible light, characterized in that the TiO 2 sol is co-precipitated with a metal solution mixed with a metal mixture such as ZnO, AgO, CuO and a binder.

가시광선 광촉매는 형광등이나 전열등의 가시광선이나 태양에너지의 자외선을 받으면 자신이 지니고 있는 전자로 채워진 가전자대(valenece band)로부터 전자가 비어있는 전도대(conduction band)로 전자가 이동하며 여기된다. 즉, 에너지를 받으면 활성이 높은 물질을 만들어 강력한 산화력을 지닌 Hydroxyl Radical(·OH)을 생성시켜 미생물을 살균하고 포름알데하이드, 페놀, TCE 등과 같은 독성 및 휘발성 유기화합물(VOC)을 산화 분해시킨다.Visible light photocatalyst is excited when visible light such as fluorescent light or electric heat or ultraviolet rays of solar energy moves from valence band filled with electrons to its own conduction band. In other words, upon receiving energy, it forms a highly active substance to produce Hydroxyl Radical (· OH) with strong oxidizing power to sterilize microorganisms and to oxidatively decompose toxic and volatile organic compounds (VOCs) such as formaldehyde, phenol, and TCE.

미생물을 살균하는 방법은 TiO2가 밴드갭(bandgap) 이상의 에너지를 받으면 전자가 하나 이동하여 전자-정공쌍이 생성되고 이것이 물, 공기중의 산소와 반응하여 H2O2, OH 등이 생성되고 이것들에 의한 강력한 살균 효과가 있다. 생성된 H2O2, OH 등에 의해 미생물의 살균되거나 유기물질의 분해가 이루어지면 CO2나 H2O로 전환되어 반도체표면에서 외부로 이용하고 다시 빛에너지를 받으면 광촉매의 기능을 수행하게 된다.The method of sterilizing microorganisms is that when TiO 2 receives energy above the bandgap, electrons move one by one to form electron-hole pairs, which react with water and oxygen in the air to produce H 2 O 2 , OH, etc. There is a strong sterilization effect. When the microorganism is sterilized or the organic material is decomposed by the generated H 2 O 2 , OH, etc., it is converted to CO 2 or H 2 O to be used externally on the surface of the semiconductor and receives light energy to perform a photocatalyst function.

종래 기술로 태양광에너지나 자외선의 에너지를 받으면 산화력을 지닌 Hydroxyl Radical(·OH)을 생성시켜 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 광촉매에 관한 것은 다수 알려져 있으나, 형광등이나 전열등의 가시광선에서 공기나 건축관련 자재의 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 가시광선 광촉매에 관한 것은 알려져 있지 않다.Conventional techniques for photocatalysts that produce oxidizing Hydroxyl Radicals (· OH) to receive microorganisms or remove formaldehyde and volatile organic substances (VOCs) are known in the prior art. There is no known visible light photocatalyst that sterilizes microorganisms of air or building materials from visible light such as electric heating lights or removes formaldehyde and volatile organic substances (VOC).

이에 본 발명자들은 태양광에너지나 자외선이 아닌 형광등이나 전열등의 가시광선에서 공기나 건축관련 자재의 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 가시광선 광촉매를 개발하고자 예의 노력한 결과, 본 발명을 완성하게 되었다.Accordingly, the present inventors have made efforts to develop visible light photocatalysts that sterilize microorganisms of air or construction-related materials or remove formaldehyde and volatile organic substances (VOC) from visible light such as fluorescent light or electric heat, not solar energy or ultraviolet light. The present invention has been completed.

결국, 본 발명의 주된 목적은 태양광선이 들어가지 않고 형광등이나 전열등을 사용하는 실내의 공기나 벽지, 장식장등에 사용하여 미생물을 살균하고 포름알데하이드와 휘발성유기화합물을 분해제거하는 특성을 갖는 가시광선 광촉매졸 및 그 제조방법을 제공하는데 있다.As a result, the main object of the present invention is visible light having the characteristics of sterilizing microorganisms and decomposing and removing formaldehyde and volatile organic compounds by using in indoor air, wallpaper, and decorative room using fluorescent light or electric heat without sunlight. It is to provide a photocatalyst sol and a method of manufacturing the same.

본 발명의 다른 목적은 태양광선이 들어가지 않고 형광등이나 전열등을 사용하는 실내의 공기나 벽지, 장식장등에 사용하여 향기를 발하면서 미생물을 살균하고 포름알데하이드와 휘발성유기화합물을 분해제거하는 특성을 갖는 향기나는 가시광선 광촉매졸 및 그 제조방법을 제공하는데 있다.It is another object of the present invention to have a characteristic of disinfecting microorganisms and decomposing and removing formaldehyde and volatile organic compounds while emitting fragrance by using in indoor air, wallpaper, and decorative room using fluorescent light or electric heat without sunlight. It is to provide a fragrant visible light photocatalyst sol and a method for producing the same.

상기 목적을 달성하기 위하여, 본 발명은 (a) 광촉매제인 티타늄 이소프로폭사이드(Ti(OCH(CH3)2)4)를 유기용매에 용해시키는 단계; (b) 상기 광촉매제가 용해된 유기용매에 증류수를 첨가한 다음, 강산을 첨가하면서 반응시켜 TiO2광촉매졸을 수득하는 단계; 및 (c) ZnO, AgO 및 CuO로 구성된 군에서 선택되는 하나 이상의 금속혼합물을 산에 용해시킨 용액과 바인더를 유기용매에 혼합시킨 용액을 1:1~1:5의 비율로 혼합한 다음, 상기 TiO2광촉매 졸과 공침하여 가시광선에 의해 활성화되는 광촉매졸을 수득하는 단계를 포함하는 형광등이나 전열등의 가시광선영역에서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 가시광선 광촉매의 제조방법을 제공한다.In order to achieve the above object, the present invention comprises the steps of (a) dissolving titanium isopropoxide (Ti (OCH (CH 3 ) 2 ) 4 ) as a photocatalyst in an organic solvent; (b) adding distilled water to the organic solvent in which the photocatalyst is dissolved, and then reacting with addition of a strong acid to obtain a TiO 2 photocatalyst sol; And (c) a solution in which at least one metal mixture selected from the group consisting of ZnO, AgO and CuO is dissolved in an acid, and a solution in which a binder is mixed with an organic solvent are mixed at a ratio of 1: 1 to 1: 5, and then Visible photocatalyst which sterilizes microorganisms or removes formaldehyde and volatile organic substance (VOC) in the visible region, such as fluorescent or electric heating lamp, by co-precipitating with TiO 2 photocatalyst sol to obtain photocatalyst sol activated by visible light. It provides a method of manufacturing.

본 발명은 또한, 상기 방법에 의해 제조되고, TiO2광촉매 졸에 금속혼합물이 공침되어 있는 가시광선에 의해 활성화되는 광촉매를 제공한다.The present invention also provides a photocatalyst prepared by the above method and activated by visible light in which a metal mixture is co-precipitated in a TiO 2 photocatalyst sol.

본 발명은 또한, 상기 가시광선에 의해 활성화되는 광촉매를 벽지, 장식장, 플라스틱, 유리, 폴리프로필렌, 인공꽃, 커튼, 섬유, 세제, 포장지 또는 건축자재에 살포, 도포 또는 디핑하는 것을 특징으로 하는 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 방법을 제공한다.The present invention also sterilizes, characterized in that spraying, coating or dipping the photocatalyst activated by the visible light on the wallpaper, decorative cabinet, plastic, glass, polypropylene, artificial flowers, curtains, fibers, detergents, wrapping paper or building materials It also provides a method for removing formaldehyde and volatile organic substances (VOC).

본 발명은 또한, (a) 광촉매제인 티타늄 이소프로폭사이드(Ti(OCH(CH3)2)4)를 유기용매에 용해시키는 단계; (b) 상기 광촉매제가 용해된 유기용매에 증류수를 첨가한 다음, 강산을 첨가하면서 반응시켜 TiO2광촉매졸을 수득하는 단계; (c) ZnO, AgO 및 CuO로 구성된 군에서 선택되는 하나 이상의 금속혼합물을 산에 용해시킨 용액과 바인더를 유기용매에 혼합시킨 용액을 1:1~1:5의 비율로 혼합한 다음, 상기 TiO2광촉매 졸과 공침하여 가시광선에 의해 활성화되는 광촉매졸을 수득하는 단계; 및 (d) 향기물질을 유기용매에 용해시킨 다음, 상기 가시광선에 의해 활성화되는 광촉매졸과 혼합반응시켜 향기나는 가시광선 광촉매를 수득하는 단계를 포함하는 형광등이나 전열등의 가시광선영역에서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 향기나는 가시광선 광촉매의 제조방법을 제공한다.The present invention also comprises the steps of (a) dissolving titanium isopropoxide (Ti (OCH (CH 3 ) 2 ) 4 ) as a photocatalyst in an organic solvent; (b) adding distilled water to the organic solvent in which the photocatalyst is dissolved, and then reacting with addition of a strong acid to obtain a TiO 2 photocatalyst sol; (c) a solution in which at least one metal mixture selected from the group consisting of ZnO, AgO, and CuO is dissolved in an acid and a solution in which a binder is mixed with an organic solvent are mixed at a ratio of 1: 1 to 1: 5, and then the TiO further comprising: 2 a photocatalyst sol with co-precipitation to obtain a photocatalyst sol which is activated by visible light; And (d) dissolving the fragrance material in an organic solvent and then mixing and reacting the photocatalyst with the photocatalyst activated by the visible light to obtain a fragrant visible light photocatalyst. Provided is a method for preparing an aromatic visible light photocatalyst which sterilizes or removes formaldehyde and volatile organic substances (VOC).

본 발명에 있어서, 상기 향기물질은 오이향, 레몬향, 레몬라임향, 복숭아향, 딸기향, 사과향, 포도향, 체리향, 바닐라향, 모과향, 유자향, 오렌지향, 장미향, 로즈마리향, 솔향, 허브향, 포퓨리향, 아카시아향, 후리지아향, 후로랄향, 라일락향, 백합향, 숲향, 헤즐럿향, 민트향, 풀꽃향, 라벤더향, 박하향, 녹차향 및 자스민향으로 구성된 군에서 선택되는 하나 또는 2 이상의 혼합물인 것을 특징으로 할 수 있다.In the present invention, the fragrance material is cucumber flavor, lemon flavor, lemon lime flavor, peach flavor, strawberry flavor, apple flavor, grape flavor, cherry flavor, vanilla flavor, quince flavor, citron flavor, orange flavor, rose flavor, rosemary flavor, Select from the group consisting of brush, herb, potpourri, acacia, freesia, floral, lilac, lily, forest, hazelt, mint, grass, lavender, peppermint, green tea and jasmine It may be characterized in that one or a mixture of two or more.

본 발명은 또한, 상기 제조방법에 의해 얻어지고, 오이향, 레몬향, 레몬라임향, 복숭아향, 딸기향, 사과향, 포도향, 체리향, 바닐라향, 모과향, 유자향, 오렌지향, 장미향, 로즈마리향, 솔향, 허브향, 포퓨리향, 아카시아향, 후리지아향, 후로랄향, 라일락향, 백합향, 숲향, 헤즐럿향, 민트향, 풀꽃향, 라벤더향, 박하향, 녹차향 및 자스민향으로 구성된 군에서 선택되는 하나 이상의 향기물질이 가시광선에 의해 활성화되는 광촉매에 함침되어 있는 향기나는 가시광선 광촉매를 제공한다.The present invention is also obtained by the above production method, cucumber flavor, lemon flavor, lemon lime flavor, peach flavor, strawberry flavor, apple flavor, grape flavor, cherry flavor, vanilla flavor, quince flavor, citron flavor, orange flavor, rose flavor , Rosemary, brush, herb, potpourri, acacia, freesia, floral, lilac, lily, forest, hazel, mint, green, lavender, peppermint, green tea and jasmine One or more fragrance materials selected from the group consisting of provide a fragrant visible light photocatalyst impregnated in the photocatalyst activated by visible light.

본 발명은 또한, 상기 향기나는 가시광선 광촉매를 벽지, 장식장, 플라스틱, 유리, 폴리프로필렌, 인공꽃, 커튼, 섬유, 세제, 포장지 또는 건축자재에 살포, 도포 또는 디핑하는 것을 특징으로 하는 향기를 발하면서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 방법을 제공한다.The present invention also provides a fragrance, characterized in that spraying, coating or dipping the scented visible light photocatalyst on wallpaper, decoration, plastic, glass, polypropylene, artificial flowers, curtains, fibers, detergents, packaging or building materials It also provides a way to sterilize microorganisms or remove formaldehyde and volatile organics (VOC).

본 발명에 있어서, 상기 바인더는 테트라에틸오르토실리케이트(TEOS) 및/또는 아미노프로필트리에폭실실란인 것을 특징으로 할 수 있다.In the present invention, the binder may be tetraethylorthosilicate (TEOS) and / or aminopropyltriepoxysilane.

본 발명의 가시광선에 의해 활성화되는 광촉매(가시광선 광촉매)는 본 발명자들이 특허를 받은 광촉매졸(등록특허 10-0405375)에 ZnO, AgO 및 CuO을 함유하는 금속혼합물과 바인더를 공침한 것이고, 향기나는 가시광선 광촉매는 상기 가시광선 광촉매에 상기한 향기물질을 일정농도 함침한 것으로 가시광선에서도 미생물을 살균할 뿐만 아니라, 기존의 광촉매에 비하여 포름알데하이드와 휘발성 유기물질(VOC)과 비슷한 제거효율을 가지고 있다.The photocatalyst (visible photocatalyst) activated by the visible light of the present invention is a co-precipitated metal mixture and binder containing ZnO, AgO and CuO in the patented photocatalyst sol (Patent 10-0405375) I visible light photocatalyst is impregnated with a certain concentration of the above-mentioned fragrance material in the visible light photocatalyst not only sterilize microorganisms in visible light, but also has a similar removal efficiency to formaldehyde and volatile organic substances (VOC) compared to conventional photocatalysts have.

이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not to be construed as being limited by these examples.

실시예 1. 가시광선 광촉매의 제조Example 1 Preparation of Visible Light Photocatalyst

광촉매제인 티타늄 이소프로폭사이드(Ti(OCH(CH3)2)4) 0.01~100ml을 에틸알코올 10~1000ml에 용해시킨 다음, 증류수를 1~100L를 첨가한 후, 질산 또는 황산을 소량(0.1~10ml/L) 첨가하면서 2~48시간 반응시켜 TiO2광촉매졸을 제조하였다. Zn, Ag, Cu 등의 금속 또는 그 혼합물 0.001mg~100g을 산 1L에 용해시킨 용액과, 테트라에틸오르토실리케이트(TEOS)와 아미노프로필트리에폭실실란을 각각 1~100ml/L로 에틸알코올에 용해시킨 용액을 1:1~1:5의 비율로 혼합한 다음, 이를 상기 TiO2광촉매졸에 상온에서 공침하여 가시광선 광촉매졸을 제조하였다.0.01 to 100 ml of titanium isopropoxide (Ti (OCH (CH 3 ) 2 ) 4 ), a photocatalyst, is dissolved in 10 to 1000 ml of ethyl alcohol, and then 1 to 100 L of distilled water is added. TiO 2 photocatalyst sol was prepared by reacting for 2 hours to 48 hours while adding ˜10 ml / L). A solution in which 0.001 mg to 100 g of a metal such as Zn, Ag, Cu or a mixture thereof was dissolved in 1 L of acid, and tetraethyl orthosilicate (TEOS) and aminopropyltriepoxysilane were dissolved in ethyl alcohol at 1 to 100 ml / L, respectively. The solution was mixed in a ratio of 1: 1 to 1: 5, and then co-precipitated in the TiO 2 photocatalyst at room temperature to prepare a visible light photocatalyst.

실시예 2. 향기나는 가시광선 광촉매의 제조Example 2 Preparation of Aromatic Visible Light Photocatalyst

오이향, 레몬향, 레몬라임향, 복숭아향, 딸기향, 사과향, 포도향, 체리향,바닐라향, 모과향, 유자향, 오렌지향, 장미향, 로즈마리향, 솔향, 허브향, 포퓨리향, 아카시아향, 후리지아향, 후로랄향, 라일락향, 백합향, 숲향, 헤즐럿향, 민트향, 풀꽃향, 라벤더향, 박하향, 녹차향 및 자스민향으로 구성된 군에서 선택되는 하나 이상의 향기물질 1㎍~100g을 에틸알코올 1.0L에 녹인 다음, 실시예 1에서 제조된 가시광선 광촉매졸과 2~48시간동안 상온에서 혼합하여 향기나는 가시광선 광촉매를 제조하였다.Cucumber flavor, lemon flavor, lemon lime flavor, peach flavor, strawberry flavor, apple flavor, grape flavor, cherry flavor, vanilla flavor, quince flavor, citron flavor, orange flavor, rose flavor, rosemary flavor, brush flavor, herbal flavor, potpourri flavor, 1 µg to 100 g of at least one fragrance material selected from the group consisting of acacia, freesia, floral, lilac, lily, forest, hazelt, mint, herb, lavender, peppermint, green tea and jasmine Was dissolved in 1.0 L of ethyl alcohol, and then mixed with the visible light photocatalyst sol prepared in Example 1 at room temperature for 2 to 48 hours to prepare a fragrant visible light photocatalyst.

본 발명에 있어서, 향기물질은 과일향으로 오이향, 레몬향, 레몬라임향, 복숭아향, 딸기향, 사과향, 포도향, 체리향, 바닐라향, 모과향, 유자향, 오렌지향이 바람직하고, 꽃향기로는 장미향, 로즈마리향, 솔향, 허브향, 포퓨리향, 아카시아향, 후리지아향, 후로랄향, 라일락향, 백합향, 숲향, 헤즐럿향, 민트향, 풀꽃향, 라벤더향, 박하향, 녹차향, 자스민향이 바람직하나, 상기 열거된 것에 제한되는 것은 아니다.In the present invention, the fragrance material is a fruit flavor, cucumber flavor, lemon flavor, lemon lime flavor, peach flavor, strawberry flavor, apple flavor, grape flavor, cherry flavor, vanilla flavor, quince flavor, citron flavor, orange flavor, The scents are rose, rosemary, scent, herb, popuri, acacia, freesia, floral, lilac, lily, forest, hazel, mint, grass, lavender, peppermint, green tea. Jasmine is preferred, but is not limited to those listed above.

실시예 3. 가시광선 광촉매의 향균력Example 3 Antibacterial Activity of Visible Photocatalyst

본 발명에 따른 가시광선 광촉매의 향균력을 조사하였다. 각각의 미생물(Klebsieia pneumoniaeATCC 4352,Staphylococcus aureusATCC 6538,Escherichia coliATCC 25922 및 MRSA(Methicillin Resistance S. aureus) ATCC 33592)이 표 1의 초기 농도로 배양되어 있는 페트리디쉬에 실시예 1에서 제조된 가시광선 광촉매를 스프레이로 1회 살포(약 0.02ml)한 다음, 35oC의 배양기에서 24시간 150회/분으로 진탕 배양 후 균수를 측정하였다.The antibacterial activity of the visible light photocatalyst according to the present invention was investigated. Spines prepared in Example 1 in Petri dishes in which each microorganism ( Klebsieia pneumoniae ATCC 4352, Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 25922 and MRSA (Methicillin Resistance S. aureus) ATCC 33592) was incubated at the initial concentration of Table 1 The photocatalyst was sprayed once with a spray (about 0.02 ml), and the number of bacteria was measured after shaking culture at 150 / min for 24 hours in a 35 ° C. incubator.

항균시험 결과,Klebsieia pneumoniaeATCC 4352는 초기농도가 5.5 x 106이었으나, 24시간후에는 1.1 x 104마리이하로,Staphylococcus aureusATCC 6538은 초기농도 6.7 x 106에서 24시간후에는 10마리이하로,Escherichia coliATCC 25922는 초기농도 7.4 x 106에서 24시간후에는 10마리이하로, MRSA(Methicillin ResistanceS.aureus) ATCC 33592는 초기농도 6.6 x 106에서 24시간후에는 10마리이하로 감소하였다.Klebsieia pneumoniaeATCC 4352의 경우에는 99.8%, 나머지 균주의 경우에는 99.99%의 제거효율을 나타냈다 (표 1).The antimicrobial test results showed that Klebsieia pneumoniae ATCC 4352 had an initial concentration of 5.5 x 10 6, but after 24 hours was less than 1.1 x 10 4 , and Staphylococcus aureus ATCC 6538 had an initial concentration of 6.7 x 10 6 and less than 10 after 24 hours. , Escherichia coli ATCC 25922 decreased to less than 10 animals after 24 hours at initial concentration of 7.4 x 10 6 , and MRSA (Methicillin Resistance S. aureus ) ATCC 33592 decreased to 10 animals after 24 hours at initial concentration of 6.6 x 10 6 . . Removal efficiency was 99.8% for Klebsieia pneumoniae ATCC 4352 and 99.99% for the remaining strains (Table 1).

미생물microbe 초기농도Initial concentration 24시간 후 농도Concentration after 24 hours Klebsieia pneumoniaeATCC 4352 Klebsieia pneumoniae ATCC 4352 5.5 x 106 5.5 x 10 6 1.1 x 104 1.1 x 10 4 Staphylococcus aureusATCC 6538 Staphylococcus aureus ATCC 6538 6.7 x 106 6.7 x 10 6 10 or less10 or less E. coliATCC 25922 E. coli ATCC 25922 7.4 x 106 7.4 x 10 6 10 or less10 or less Methicillin ResistanceS. aureusATCC 33592Methicillin Resistance S. aureus ATCC 33592 6.6 x 106 6.6 x 10 6 10 or less10 or less

실시예 4. 향기나는 가시광선 광촉매의 향균력Example 4 Antibacterial Activity of Aromatic Visible Light Photocatalyst

본 발명에 따른 향기나는 가시광선 광촉매의 향균력을 조사하였다. 각각의 미생물(Klebsieia pneumoniaeATCC 4352,Staphylococcus aureusATCC 6538,Escherichia coliATCC 25922 및 MRSA(Methicillin Resistance S. aureus) ATCC33592)이 표 2의 초기 농도로 배양되어 있는 페트리디쉬에 실시예 2에서 제조된 향기나는 가시광선 광촉매를 스프레이로 1회 살포(약 0.02ml)한 다음, 35oC의 배양기에서 24시간 150회/분으로 진탕 배양 후 균수를 측정하였다.The antibacterial activity of the fragrant visible light photocatalyst according to the present invention was investigated. Each microorganism ( Klebsieia pneumoniae ATCC 4352, Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 25922 and MRSA (Methicillin Resistance S. aureus) ATCC33592) was scented in Petri dishes prepared in Example 2 in Petri dishes. The visible light photocatalyst was sprayed once (about 0.02 ml), and the number of bacteria was measured after shaking culture at 150 times / min for 24 hours in a 35 ° C. incubator.

항균시험 결과,Klebsieia pneumoniaeATCC 4352는 초기농도 5.5 x 106에서 24시간후에는 1.1 x 104마리이하로,Staphylococcus aureusATCC 6538은 초기농도 6.7 x 106에서 24시간후에는 1.3 x 104마리이하로,Escherichia coliATCC 25922는 초기농도 7.4 x 106에서 24시간후에는 1.5 x 104마리이하로, MRSA(Methicillin ResistanceS.aureus) ATCC 33592는 초기농도 6.6 x 106에서 24시간후에는 10마리이하로 감소하였다.Klebsieia pneumoniaeATCC 4352,Staphylococcus aureusATCC 6538 및Escherichia coliATCC 25922의 경우에는 99.8%, Methicillin ResistanceS. aureusATCC 33592의 경우에는 99.99%의 제거효율을 나타냈다 (표 2).The antimicrobial test showed that Klebsieia pneumoniae ATCC 4352 was 1.1 x 10 4 or less after 24 hours at an initial concentration of 5.5 x 10 6 , and Staphylococcus aureus ATCC 6538 was 1.3 x 10 4 or less after 24 hours at an initial concentration of 6.7 x 10 6 . Escherichia coli ATCC 25922 is less than 1.5 x 10 4 animals after 24 hours at initial concentration of 7.4 x 10 6 , and 10 mice after 24 hours at initial concentration of 6.6 x 10 6 at MRSA (Methicillin Resistance S. aureus ) ATCC 33592 Decreased below. The removal efficiencies of Klebsieia pneumoniae ATCC 4352, Staphylococcus aureus ATCC 6538 and Escherichia coli ATCC 25922 were 99.8% and 99.99% for Methicillin Resistance S. aureus ATCC 33592 (Table 2).

미생물microbe 초기농도Initial concentration 24시간 후 농도Concentration after 24 hours Klebsieia pneumoniaeATCC 4352 Klebsieia pneumoniae ATCC 4352 5.5 x 106 5.5 x 10 6 1.1 x 104 1.1 x 10 4 Staphylococcus aureusATCC 6538 Staphylococcus aureus ATCC 6538 6.7 x 106 6.7 x 10 6 1.3 x 104 1.3 x 10 4 E. coliATCC 25922 E. coli ATCC 25922 7.4 x 106 7.4 x 10 6 1.5 x 104 1.5 x 10 4 Methicillin ResistanceS. aureusATCC 33592Methicillin Resistance S. aureus ATCC 33592 6.6 x 106 6.6 x 10 6 10 or less10 or less

실시예 5. 가시광선 광촉매의 포름알데하이드 및 암모니아 분해능Example 5 Formaldehyde and Ammonia Degradation of Visible Photocatalyst

본 발명에 따른 가시광선 광촉매의 포름알데하이드 분해능과 암모니아 탈취율을 조사하였다. 2L 용기에 암모니아를 넣고 실시예 1에서 제조된 가시광선 광촉매를 0.5ml 분무한 다음, 20W/의 형광등에서 암모니아의 탈취율 및 포름알데히드의 분해율을 분석하였다. 그 결과, 암모니아는 5분 및 60분 후에 각각 50.0% 및 57.6% 탈취되었으며, 포름알데히드는 5분 및 60분 후에 각각 60.0% 및 70.8% 분해되었다. 일본산 광촉매(일본 요시까와 종합개발 광촉매수용액 TPX85)를 같은 조건으로 사용여 실험한 결과, 암모니아의 탈취율은 5분 및 60분 후에 각각 50.0% 및 56.1%이었고, 포름알데히드 분해율은 5분 및 60분후에 각각 60.0% 및 69.2%이었다. 결국 본 발명에 따른 가시광선 광촉매는 기존의 태양광이나 자외선을 이용하는 광촉매와 탈취효율이 비슷한 것으로 나타났다.Formaldehyde resolution and ammonia deodorization rate of the visible light photocatalyst according to the present invention were investigated. Ammonia was put in a 2 L container, and 0.5 ml of the visible light photocatalyst prepared in Example 1 was sprayed, and then the deodorization rate of ammonia and the decomposition rate of formaldehyde were analyzed in a fluorescent lamp of 20 W /. As a result, ammonia deodorized 50.0% and 57.6% after 5 and 60 minutes, respectively, and formaldehyde decomposed 60.0% and 70.8% after 5 and 60 minutes, respectively. Experiments using a Japanese photocatalyst (Yoshikawa Japan Developed Photocatalytic Solution TPX85) under the same conditions showed that the deodorization rates of ammonia were 50.0% and 56.1% after 5 and 60 minutes, respectively, and the rate of formaldehyde decomposition was 5 and 60 minutes, respectively. After minutes were 60.0% and 69.2%, respectively. As a result, the visible light photocatalyst according to the present invention was found to have a similar deodorization efficiency with a photocatalyst using conventional sunlight or ultraviolet light.

실시예 6. 향기나는 가시광선 광촉매의 포름알데하이드 및 암모니아 분해능Example 6 Formaldehyde and Ammonia Degradation of Aromatic Visible Light Photocatalyst

본 발명에 따른 향기나는 가시광선 광촉매의 포름알데하이드 분해능과 암모니아 탈취율을 조사하였다. 2L 용기에 암모니아를 넣고 실시예 2에서 제조된 향기나는 가시광선 광촉매를 0.5ml 분무한 다음, 형광등 조사 조건에서, 암모니아의 탈취율 및 포름알데히드의 분해율을 분석하였다. 그 결과, 암모니아는 5분 및 60분 후에 각각 51.1% 및 53.0% 탈취되었으며, 포름알데히드는 5분 및 60분 후에 각각 58.7% 및 65.0% 분해되었다. 결국 본 발명에 따른 향기나는 가시광선 광촉매는 기존의 태양광이나 자외선을 이용하는 광촉매나 실시예 1에 따른 가시광선 광촉매와 탈취효율이 비슷한 것으로 나타났다.Formaldehyde resolution and ammonia deodorization rate of the fragrant visible light photocatalyst according to the present invention were investigated. Ammonia was put in a 2 L container, and 0.5 ml of the fragrant visible light photocatalyst prepared in Example 2 was sprayed, and the deodorization rate of ammonia and the decomposition rate of formaldehyde were analyzed under fluorescent lamp irradiation conditions. As a result, ammonia deodorized 51.1% and 53.0% after 5 and 60 minutes, respectively, and formaldehyde decomposed 58.7% and 65.0% after 5 and 60 minutes, respectively. As a result, the fragrant visible light photocatalyst according to the present invention was found to have a similar deodorization efficiency to the photocatalyst using the conventional sunlight or ultraviolet light or the visible light photocatalyst according to Example 1.

이상으로 본 발명 내용의 특정한 부분을 상세히 기술하였는 바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의하여 정의된다고 할 것이다.Having described the specific part of the present invention in detail, it is obvious to those skilled in the art that such a specific description is only a preferred embodiment, thereby not limiting the scope of the present invention. something to do. Thus, the substantial scope of the present invention will be defined by the appended claims and their equivalents.

상기와 같이 본 발명에 따른 가시광선 광촉매 및 향기나는 가시광선 광촉매 는 형광등이나 전열등의 가시광선영역에서 광촉매기능인 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 효율적으로 제거할 수 있다. 본 발명에 따른 가시광선 광촉매 및 향기나는 가시광선 광촉매는 벽지나 장식장, 플라스틱, 폴리프로필렌 등의 인조물질, 커튼, 섬유, 세제, 포장지, 건축자재 등에 살포하여 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 데 유용하다.As described above, the visible light photocatalyst and the fragrant visible light photocatalyst may sterilize microorganisms having a photocatalytic function in the visible light region such as fluorescent lamps or heat transfer lamps or efficiently remove formaldehyde and volatile organic substances (VOC). Visible light photocatalyst and fragrant visible light photocatalyst according to the present invention is applied to artificial materials such as wallpaper, decorative cabinet, plastic, polypropylene, curtains, textiles, detergents, wrapping paper, building materials, etc. to sterilize microorganisms or formaldehyde and volatile organic materials. Useful for removing (VOC).

Claims (7)

다음의 단계를 포함하는 형광등이나 전열등의 가시광선영역에서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 가시광선 광촉매졸의 제조방법:Method for preparing visible photocatalyst which disinfects microorganisms or removes formaldehyde and volatile organic substances (VOC) in the visible region of a fluorescent or electric heating lamp comprising the following steps: (a) 광촉매제인 티타늄 이소프로폭사이드(Ti(OCH(CH3)2)4)를 유기용매에 용해시키는 단계;(a) dissolving titanium isopropoxide (Ti (OCH (CH 3 ) 2 ) 4 ) as a photocatalyst in an organic solvent; (b) 상기 광촉매제가 용해된 유기용매에 증류수를 첨가한 다음, 강산을 첨가하면서 반응시켜 TiO2광촉매졸을 수득하는 단계; 및(b) adding distilled water to the organic solvent in which the photocatalyst is dissolved, and then reacting with addition of a strong acid to obtain a TiO 2 photocatalyst sol; And (c) AgO 및/또는 CuO의 금속혼합물을 산에 용해시킨 용액과 바인더를 유기용매에 혼합시킨 용액을 1:1~1:5의 비율로 혼합한 다음, 상기 TiO2광촉매 졸과 공침하여 가시광선에 의해 활성화되는 광촉매졸을 수득하는 단계.(c) a solution in which a metal mixture of AgO and / or CuO is dissolved in an acid and a mixture of a binder and an organic solvent are mixed at a ratio of 1: 1 to 1: 5, and then co-precipitated with the TiO 2 photocatalyst sol to make visible Obtaining a photocatalyst sol activated by light. 삭제delete 다음의 단계를 포함하는 형광등이나 전열등의 가시광선영역에서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 향기나는 가시광선 광촉매의 제조방법:A method for producing a fragrant visible light photocatalyst which sterilizes microorganisms or removes formaldehyde and volatile organic substances (VOC) in the visible light region of a fluorescent or electric heating lamp comprising the following steps: (a) 광촉매제인 티타늄 이소프로폭사이드(Ti(OCH(CH3)2)4)를 유기용매에 용해시키는 단계;(a) dissolving titanium isopropoxide (Ti (OCH (CH 3 ) 2 ) 4 ) as a photocatalyst in an organic solvent; (b) 상기 광촉매제가 용해된 유기용매에 증류수를 첨가한 다음, 강산을 첨가하면서 반응시켜 TiO2광촉매졸을 수득하는 단계;(b) adding distilled water to the organic solvent in which the photocatalyst is dissolved, and then reacting with addition of a strong acid to obtain a TiO 2 photocatalyst sol; (c) AgO 및/또는 CuO의 금속혼합물을 산에 용해시킨 용액과 바인더를 유기용매에 혼합시킨 용액을 1:1~1:5의 비율로 혼합한 다음, 상기 TiO2광촉매 졸과 공침하여 가시광선에 의해 활성화되는 광촉매졸을 수득하는 단계; 및(c) a solution in which a metal mixture of AgO and / or CuO is dissolved in an acid and a mixture of a binder and an organic solvent are mixed at a ratio of 1: 1 to 1: 5, and then co-precipitated with the TiO 2 photocatalyst sol to make visible Obtaining a photocatalyst sol activated by light; And (d) 오이향, 레몬향, 레몬라임향, 복숭아향, 딸기향, 사과향, 포도향, 체리향, 바닐라향, 모과향, 유자향, 오렌지향, 장미향, 로즈마리향, 솔향, 허브향, 포퓨리향, 아카시아향, 후리지아향, 후로랄향, 라일락향, 백합향, 숲향, 헤즐럿향, 민트향, 풀꽃향, 라벤더향, 박하향, 녹차향 및 자스민향으로 구성된 군에서 선택되는 하나 또는 2 이상의 천연물 향기물질을 유기용매에 용해시킨 다음, 상기 가시광선에 의해 활성화되는 광촉매졸과 혼합반응시켜 향기나는 가시광선 광촉매를 수득하는 단계.(d) Cucumber, lemon, lemon lime, peach, strawberry, apple, grape, cherry, vanilla, quince, citron, orange, rose, rosemary, pine, herb, herbal One, two or more natural products selected from the group consisting of fury, acacia, freesia, floral, lilac, lily, forest, hazelt, mint, grass, lavender, mint, green tea and jasmine Dissolving the fragrance substance in an organic solvent and then mixing and reacting with the photocatalyst sol activated by the visible ray to obtain a fragrant visible ray photocatalyst. 삭제delete 삭제delete 제1항의 가시광선에 의해 활성화되는 실내자재 도포용 광촉매를 벽지, 장식장, 플라스틱, 유리, 폴리프로필렌, 인공꽃, 커튼, 섬유, 세제, 포장지 또는 건축자재에 살포, 도포 또는 디핑하는 것을 특징으로 하는 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 방법.Spraying, coating or dipping the photocatalyst for indoor materials activated by the visible light of claim 1 to wallpaper, decoration, plastic, glass, polypropylene, artificial flowers, curtains, fibers, detergents, wrapping paper or building materials Sterilization or removal of formaldehyde and volatile organics (VOCs). 제3항의 실내자재 도포용 향기나는 가시광선 광촉매를 벽지, 장식장, 플라스틱, 유리, 폴리프로필렌, 인공꽃, 커튼, 섬유, 세제, 포장지 또는 건축자재에 살포, 도포 또는 디핑하는 것을 특징으로 하는 향기를 발하면서 미생물을 살균하거나 포름알데하이드와 휘발성 유기물질(VOC)을 제거하는 방법.The fragrance is characterized by spraying, coating or dipping the fragrant visible light photocatalyst for coating the interior materials of claim 3 to wallpaper, decor, plastic, glass, polypropylene, artificial flowers, curtains, fibers, detergents, wrapping paper or building materials. A method of killing microorganisms or removing formaldehyde and volatile organic substances (VOCs) while firing.
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