JP2006297230A - Titanium oxide thin film, titanium oxide thin film-containing photocatalytic material, its manufacturing method, apparatus for cleaning water by using photocatalyst, and method for cleaning water by using photocatalytic reaction - Google Patents
Titanium oxide thin film, titanium oxide thin film-containing photocatalytic material, its manufacturing method, apparatus for cleaning water by using photocatalyst, and method for cleaning water by using photocatalytic reaction Download PDFInfo
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- JP2006297230A JP2006297230A JP2005120215A JP2005120215A JP2006297230A JP 2006297230 A JP2006297230 A JP 2006297230A JP 2005120215 A JP2005120215 A JP 2005120215A JP 2005120215 A JP2005120215 A JP 2005120215A JP 2006297230 A JP2006297230 A JP 2006297230A
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- Prior art keywords
- titanium oxide
- manufacturing
- photocatalytic
- oxide film
- suspension
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 126
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 124
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000000463 material Substances 0.000 title claims abstract description 37
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000013032 photocatalytic reaction Methods 0.000 title claims description 6
- 239000011941 photocatalyst Substances 0.000 title abstract description 30
- 239000010409 thin film Substances 0.000 title abstract description 12
- 238000004140 cleaning Methods 0.000 title abstract 3
- 239000000725 suspension Substances 0.000 claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 238000004070 electrodeposition Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 47
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 31
- 238000001652 electrophoretic deposition Methods 0.000 claims description 28
- 239000002904 solvent Substances 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- 238000000746 purification Methods 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 20
- 239000004020 conductor Substances 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 15
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 150000001491 aromatic compounds Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 71
- 239000011248 coating agent Substances 0.000 abstract description 19
- 238000000576 coating method Methods 0.000 abstract description 19
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- 239000010936 titanium Substances 0.000 abstract description 5
- 229910052719 titanium Inorganic materials 0.000 abstract description 5
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- 238000001035 drying Methods 0.000 description 7
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- 230000000052 comparative effect Effects 0.000 description 6
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- 238000010586 diagram Methods 0.000 description 5
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Images
Abstract
Description
本発明は、基体上に酸化チタン膜が成膜された光触媒材料に関し、より詳細には、導電性の基体上に粗さを有する酸化チタン膜が成膜された光触媒材料、その製造方法、その光触媒材料を含む水処理装置、および、水処理方法に関する。 The present invention relates to a photocatalytic material in which a titanium oxide film is formed on a substrate, and more specifically, a photocatalytic material in which a titanium oxide film having roughness is formed on a conductive substrate, a manufacturing method thereof, and the The present invention relates to a water treatment apparatus including a photocatalytic material and a water treatment method.
近年、酸化チタンは、紫外線照射により強い酸化力を示すことから、光触媒として、環境浄化への応用が様々な分野で検討されている。今日、酸化チタンを光触媒として利用して水や空気を浄化するシステムが数多く提案されているが、酸化チタン粉末での利用は反応後に空気や水と酸化チタン粉末とを分離するのに手間がかかるため、ほとんどの場合、酸化チタンをセラミックス系の担体に担持したフィルターを用いている。例えば、特開２００１−３８２１８号公報（特許文献１）には、セラミック多孔体の多孔質表面層に、酸化チタンを担持させてなる光触媒フィルターが開示されている。 In recent years, since titanium oxide exhibits a strong oxidizing power when irradiated with ultraviolet rays, its application to environmental purification as a photocatalyst has been studied in various fields. Today, many systems for purifying water and air using titanium oxide as a photocatalyst have been proposed, but use with titanium oxide powder takes time and effort to separate air or water from titanium oxide powder after reaction. Therefore, in most cases, a filter in which titanium oxide is supported on a ceramic carrier is used. For example, Japanese Patent Laid-Open No. 2001-38218 (Patent Document 1) discloses a photocatalytic filter in which titanium oxide is supported on a porous surface layer of a ceramic porous body.
一方、金属担体は、セラミックス担体に比べ、加工性、形状制御性およびコスト面において優れており、さらに、金属担体は、導電性を有することから、担体に適度な電位をかけることにより、光触媒反応における表面ホール濃度をあげることが可能になる。したがって、酸化チタンの担体として金属を用いることが出来れば、優れた光触媒フィルターを実現することができる。 On the other hand, the metal carrier is superior to the ceramic carrier in terms of processability, shape controllability, and cost. Furthermore, since the metal carrier has conductivity, the photocatalytic reaction can be achieved by applying an appropriate potential to the carrier. It is possible to increase the surface hole concentration at. Therefore, if a metal can be used as the carrier for titanium oxide, an excellent photocatalytic filter can be realized.
ここで、酸化物粉末の導電性担体へのコーティング手法の一つに電気泳動電着（以下ＥＰＤという）がある。この方法は、酸化物粉末が分散したサスペンションで電極に電位をかけることで、酸化物粉末を電気泳動させ、電極上に堆積する技術であり、（１）大面積へのコーティングが可能、（２）複雑形状へのコーティングが可能、（３）コーティング膜厚制御が容易、（４）安価である、といった利点を有している。しかしながら、金属担体に酸化チタンをコーティングすると、担体金属と酸化チタンとの熱膨張率の差が原因となって、焼成後にコーティング膜に多数のクラックが入ることがほとんどで、大面積均一コーティングが困難であるという問題点があった。図６は、金属メッシュ上に電気泳動電着で堆積した、従来の酸化チタン膜に焼成後発生した剥離とクラックを示す。 Here, electrophoretic electrodeposition (hereinafter referred to as EPD) is one of techniques for coating oxide powder on a conductive carrier. This method is a technique in which an oxide powder is electrophoresed by applying an electric potential to the electrode with a suspension in which the oxide powder is dispersed, and is deposited on the electrode. (1) Large area coating is possible. (2 It has the advantages of being capable of coating complex shapes, (3) easy coating film thickness control, and (4) inexpensive. However, when titanium oxide is coated on a metal carrier, the coating film is almost always cracked after firing due to the difference in thermal expansion coefficient between the carrier metal and titanium oxide, making large area uniform coating difficult. There was a problem that. FIG. 6 shows delamination and cracks generated after firing on a conventional titanium oxide film deposited by electrophoretic electrodeposition on a metal mesh.
上述したように、金属の担体は、光触媒フィルターの担体として、多くの利点と可能性を有するにもかかわらず、酸化チタンとの密着性が低いという問題のため、これまで用いられてこなかった。そこで、金属担体を用いた信頼性の高い酸化チタン光触媒フィルターを作製する技術が求められていた。 As described above, metal carriers have not been used so far due to the problem of low adhesion to titanium oxide, despite having many advantages and possibilities as photocatalytic filter carriers. Therefore, a technique for producing a highly reliable titanium oxide photocatalytic filter using a metal carrier has been demanded.
また、光触媒反応は表面反応であり、活性表面の面積がなるべく大きい方が望ましい。すなわち、コーティングは平滑であるよりも粗さを有する方が有利となる。しかしながら金属担体上に適度な粗さを有する酸化チタンコーティングを再現性良く作製する手法はこれまで得られていなかった。 The photocatalytic reaction is a surface reaction, and it is desirable that the area of the active surface is as large as possible. That is, it is advantageous for the coating to have roughness rather than smooth. However, a method for producing a titanium oxide coating having an appropriate roughness on a metal carrier with good reproducibility has not been obtained so far.
さらに加えて、今日、難分解性の発ガン性物質である、１−４ジオキサンの光触媒分解について種々検討がなされているが、１−４ジオキサンは、その中間体であるＥＧＤＦ（エチレングリコールジフォルメイト）が酸化チタンに吸着しにくいため、従来の光触媒水浄化装置では最終分解することが難しく、この様な物質を効率的に分解する方法が求められていた。さらに、その人体に対する悪影響から、ジクロロエタン、トリクロロエタンなどの含ハロゲン化合物や、各種環境ホルモンに代表される芳香族化合物などに汚染された水の有効な浄化方法が求められていた。
本発明は、上記従来技術に鑑みてなされたものであり、本発明は、金属をはじめとする導電性の基体上に、剥離やクラックの生じない信頼性の高い酸化チタン薄膜であって、光触媒として好適な粗さを有する酸化チタン薄膜を含む光触媒材料と、その製造方法を提供することを目的とする。また、本発明の他の目的は、上記光触媒材料を含む水浄化装置、および、その水浄化方法を提供することを目的とする。 The present invention has been made in view of the above prior art, and the present invention is a highly reliable titanium oxide thin film that is free from peeling or cracking on a conductive substrate including metal, and is a photocatalyst. An object of the present invention is to provide a photocatalytic material including a titanium oxide thin film having a roughness suitable for the above and a method for producing the same. Another object of the present invention is to provide a water purification device containing the photocatalytic material and a method for purifying the water.
金属担体上で酸化チタンコーティング膜にクラックを生じなくさせるためには、乾燥過程と焼成過程で生じる収縮に伴う応力をなるべく少なくする必要がある。したがって、乾燥過程でのクラック発生防止には、表面張力が水よりも小さい有機溶媒系が有利である。 In order to prevent the titanium oxide coating film from cracking on the metal carrier, it is necessary to reduce as much as possible the stress associated with the shrinkage that occurs during the drying and firing processes. Therefore, an organic solvent system having a surface tension smaller than that of water is advantageous for preventing cracks during the drying process.
また、焼成過程でのクラック発生防止には、（１）コーティング膜の膜厚を薄くすること、（２）コーティング膜自体が緻密でないこと、が重要となる。コーティング膜の表面に粗さを付与するには、成膜過程で電極近傍で何らかの不均一反応を共存させることが望ましい。酸化チタンは、イソプロピルアルコール（以下、ＩＰＡという）中で正電荷を有し、ＥＰＤでは、カソード側に泳動する。一方、ＩＰＡは、酸化チタンの酸化作用によって分解され、アセトンとプロトンを生成する。このアセトンは、カソードに十分な負電位とプロトンがあると還元されて、カソードにおいてプロパンなどのガス種を生成する。したがって、酸化チタン−ＩＰＡ系のサスペンションに、予め紫外線を照射し、酸化チタンの酸化反応によって、ＩＰＡを分解してアセトンとプロトンを生成させるか、あるいは、サスペンションに、予めアセトンと水を微量添加しておくと、ＥＰＤのカソード側で、酸化チタンの電気泳動成膜とガス発生が同時に起こり、このバランスをうまく調整するとコーティング膜の表面に適当な粗さを付与することができると考えられる。 In order to prevent the occurrence of cracks in the firing process, it is important that (1) the coating film is thin, and (2) the coating film itself is not dense. In order to impart roughness to the surface of the coating film, it is desirable that some heterogeneous reaction coexist in the vicinity of the electrode during the film formation process. Titanium oxide has a positive charge in isopropyl alcohol (hereinafter referred to as IPA) and migrates to the cathode side in EPD. On the other hand, IPA is decomposed by the oxidizing action of titanium oxide to produce acetone and protons. This acetone is reduced when there is a sufficient negative potential and proton at the cathode, and produces a gas species such as propane at the cathode. Therefore, the titanium oxide-IPA suspension is irradiated with ultraviolet rays in advance and IPA is decomposed by the oxidation reaction of titanium oxide to generate acetone and protons, or a small amount of acetone and water is added to the suspension in advance. In other words, it is considered that on the cathode side of EPD, electrophoretic film formation of titanium oxide and gas generation occur at the same time. If this balance is well adjusted, an appropriate roughness can be imparted to the surface of the coating film.
以上のような着想の下、本発明者らは、各種の酸化チタン粒子を用い、水系、有機溶媒系について、バインダーの添加の有無も含めて様々な条件で鋭意検討を実施した。その結果、所定の条件の下、紫外線照射を行った酸化チタン−ＩＰＡ系のサスペンションを用いて、金属担体にＥＰＤを行うことにより、クラックフリーであって、コーティング膜表面に光触媒として好適な粗さ備えた酸化チタン薄膜を作製することができることを見出し、本発明に至ったのである。 Under the above idea, the present inventors have conducted extensive studies on various types of titanium oxide particles under various conditions including the presence or absence of addition of a binder with respect to aqueous and organic solvent systems. As a result, by carrying out EPD on a metal carrier using a titanium oxide-IPA suspension subjected to ultraviolet irradiation under predetermined conditions, it is crack-free and has a roughness suitable as a photocatalyst on the coating film surface. The present inventors have found that a titanium oxide thin film provided can be produced, and have reached the present invention.
すなわち、本発明によれば、導電性の基体と、該基体に形成された多孔質酸化チタン膜とを含む光触媒材料が提供される。前記導電性の基体は金属製メッシュとすることができる。前記多孔質酸化チタン膜は、粒径が５ｎｍ〜２００ｎｍの酸化チタン粒子から作製されたものとすることができる。 That is, according to the present invention, a photocatalytic material including a conductive substrate and a porous titanium oxide film formed on the substrate is provided. The conductive substrate may be a metal mesh. The porous titanium oxide film may be prepared from titanium oxide particles having a particle size of 5 nm to 200 nm.
また、本発明によれば、導電性の基体上に多孔質酸化チタン膜が形成された光触媒材料を製造する方法であって、前記製造方法は、溶媒と酸化チタン粉末とからサスペンションを作製する工程と、前記サスペンションに紫外線を照射する工程と、前記紫外線を照射されたサスペンションの中で電気泳動電着を行い、前記酸化チタン粉末を前記導電性の基体上に堆積させつつガスを発生させる工程とを含む製造方法が提供される。前記製造方法は、前記酸化チタン粉末が堆積した前記基板を焼成する工程を含むことができる。前記溶媒は、イソプロピルアルコールを含む有機溶媒とすることができる。 According to the present invention, there is also provided a method for producing a photocatalytic material in which a porous titanium oxide film is formed on a conductive substrate, the method comprising producing a suspension from a solvent and titanium oxide powder. And a step of irradiating the suspension with ultraviolet light, and a step of performing electrophoretic deposition in the suspension irradiated with the ultraviolet light to generate gas while depositing the titanium oxide powder on the conductive substrate; A manufacturing method is provided. The manufacturing method may include a step of firing the substrate on which the titanium oxide powder is deposited. The solvent can be an organic solvent containing isopropyl alcohol.
さらに、本発明によれば、導電性の基体上に多孔質酸化チタン膜が形成された光触媒材料を製造する方法であって、前記製造方法は、溶媒と酸化チタン粉末とからサスペンションを作製する工程と、前記サスペンションの中で電気泳動電着を行い、前記酸化チタン粉末を前記導電性の基体上に堆積させつつ溶媒ガスを発生させる工程とを含む製造方法が提供される。前記製造方法は、前記酸化チタン粉末が堆積した前記基板を焼成する工程を含むことができる。前記溶媒は、イソプロピルアルコールおよびアセトンを含む有機溶媒とすることができる。 Furthermore, according to the present invention, there is provided a method for producing a photocatalytic material in which a porous titanium oxide film is formed on a conductive substrate, the method comprising producing a suspension from a solvent and titanium oxide powder. And a step of performing electrophoretic electrodeposition in the suspension and generating a solvent gas while depositing the titanium oxide powder on the conductive substrate. The manufacturing method may include a step of firing the substrate on which the titanium oxide powder is deposited. The solvent may be an organic solvent containing isopropyl alcohol and acetone.
前記導電性の基体は金属製メッシュとすることができる。また、前記酸化チタン粉末の粒径は５ｎｍ〜２００ｎｍとすることができる。 The conductive substrate may be a metal mesh. The titanium oxide powder may have a particle size of 5 nm to 200 nm.
本発明のさらに他の態様によれば、水槽と、該水槽の近傍に配設された紫外線発生部材と、電源と、該電源に接続されたカソード電極とアノード電極とを含む光触媒水浄化装置であって、前記電極は前記水槽の内部に配設されており、前記アノード電極は、多孔質酸化チタン膜が形成された導電性材料を含む光触媒水浄化装置が提供される。 According to still another aspect of the present invention, there is provided a photocatalytic water purification apparatus including a water tank, an ultraviolet ray generating member disposed in the vicinity of the water tank, a power source, and a cathode electrode and an anode electrode connected to the power source. The electrode is provided inside the water tank, and the anode electrode is provided with a photocatalytic water purification device including a conductive material on which a porous titanium oxide film is formed.
さらに、本発明によれば、光触媒反応を利用した水浄化方法であって、前記方法は、被浄化水の中に、多孔質酸化チタン膜が形成された導電性材料を含むアノード電極とカソード電極とを配設する工程と、前記電極間に電位差を設ける工程とを含む水浄化方法が提供される。前記電位差は、前記アノード電極の多孔質酸化チタン膜の表面ホール濃度を増加させ、前記被浄化水中に含まれる浄化対象分子を該多孔質酸化チタン膜の表面に吸着させる電位差とすることができる。前記浄化対象分子は、１−４ジオキサン、含ハロゲン化合物および芳香族化合物から選ばれるものとすることができる。 Furthermore, according to the present invention, there is provided a water purification method utilizing a photocatalytic reaction, the method comprising an anode electrode and a cathode electrode containing a conductive material in which a porous titanium oxide film is formed in the water to be purified. Is provided, and a water purification method including a step of providing a potential difference between the electrodes is provided. The potential difference may be a potential difference that increases the surface hole concentration of the porous titanium oxide film of the anode electrode and causes the molecules to be purified contained in the water to be purified to be adsorbed on the surface of the porous titanium oxide film. The molecule to be purified can be selected from 1-4 dioxane, a halogen-containing compound and an aromatic compound.
本発明によれば、金属をはじめとする導電性の基体上に、剥離やクラックの生じない信頼性の高い酸化チタン薄膜であって、光触媒として表面に好適な粗さを有する酸化チタン薄膜を含む光触媒材料を提供することができる。本発明により製造された光触媒材料は、水浄化装置における電極として使用することができ、適度な電位をかけることにより、光触媒反応における表面ホール濃度をあげることができる。さらに加えて、適度な電位をかけることにより、電子密度の高い分子が上記光触媒に好適に吸着するという効果も相まって、従来の光触媒水浄化装置では分解が困難であった物質を効率的に分解することができる。 According to the present invention, a highly reliable titanium oxide thin film that does not cause peeling or cracking on a conductive substrate such as a metal and includes a titanium oxide thin film having a suitable roughness on the surface as a photocatalyst is included. A photocatalytic material can be provided. The photocatalyst material produced according to the present invention can be used as an electrode in a water purification apparatus, and the surface hole concentration in the photocatalytic reaction can be increased by applying an appropriate potential. In addition, by applying an appropriate potential, combined with the effect that molecules with high electron density are favorably adsorbed to the photocatalyst, the material that was difficult to decompose with the conventional photocatalytic water purification device is efficiently decomposed. be able to.
以下、本発明を具体的な実施の形態をもって説明するが、本発明は、後述する実施の形態に限定されるものではない。図１は、本発明の、ＥＰＤによる酸化チタン成膜の態様を示した図である。サスペンション１０の中に、カソード電極として導電体１２が、アノードとして電極１４が浸されている。導電体１２は、ＥＰＤにおいて酸化チタンの担体となるものである。電極１４には、アルミニウム板などが適宜選択し用いることができる。導電体１２には、金属製メッシュを用いることが好ましい。具体的には、ステンレスメッシュ、チタンメッシュまたは白金メッシュ、若しくは、公知の金属製メッシュにＩｎ−Ｇａ合金をコーティングしたものなどを用いることができる。ただし、本発明においては、導電体１２を上記材料に限定するものではなく、後述する、光触媒水浄化装置の電極として用いられた場合に、酸化チタン膜との関係で、電位効果を好適に得られるような材料を適宜選択することができる。
Hereinafter, the present invention will be described with specific embodiments, but the present invention is not limited to the embodiments described below. FIG. 1 is a diagram showing an aspect of titanium oxide film formation by EPD according to the present invention. In the
サスペンション１０は、以下の手順で調整される。分散される酸化チタン粒子１６には、高純度の酸化チタン粉末が用いられることが好ましい。酸化チタン粒子１６の結晶形は、光触媒として好適なアナターゼ型のものが好ましい。酸化チタンの結晶粒子の大きさは、導電体の担体にあまり緻密に堆積しないようある程度の大きさ以上のものが好ましく、粒径で５〜２００ｎｍ、比表面積で７〜３００ｍ２／ｇ程度のものが好ましい。本発明においては、サスペンション１０に、酸化チタンのほかに他の光触媒物質を加えてＥＰＤ成膜することもできる。上記光触媒物質としては、ＳｒＴｉＯ３、ＫＴａＯ３、ＳｎＯ２、Ｎｂ２Ｏ５、ＷＯ３、Ｆｅ２Ｏ３、Ｂｉ２Ｏ３、ＦｅＴｉＯ３、ＭｎＴｉＯ３、ＢａＴｉＯ３、ＺｎＯ、Ｉｎ２Ｏ３、Ｖ２Ｏ５、ＮｂＯ２、ＣａＴｉＯ３、ＳｒＮｂ２Ｏ６、酸化ジルコニウムを挙げることができる。
The
次に、この酸化チタン粉末を、有機溶媒の中で充分に撹拌したのち、超音波によって分散させる。サスペンションの溶媒に有機溶媒系を用いることにより、その表面張力が水よりも小さいため、後の乾燥過程において、酸化チタン膜にクラックが生じにくくなる。本発明の有機溶媒は、ＩＰＡを含むことが好ましい。本発明において、ＥＰＤのサスペンションに用いられる溶媒は、乾燥過程におけるクラックを防止し、後述する、酸化チタン膜表面に粗さを生じさせる過程において、上記溶媒由来のガス種を生成することのできる溶剤を、適宜選択することができる。 Next, the titanium oxide powder is sufficiently stirred in an organic solvent and then dispersed by ultrasonic waves. By using an organic solvent system as a solvent for the suspension, the surface tension is smaller than that of water, so that cracks are less likely to occur in the titanium oxide film in the subsequent drying process. The organic solvent of the present invention preferably contains IPA. In the present invention, the solvent used in the suspension of EPD is a solvent that can prevent cracks in the drying process and generate a gas species derived from the solvent in the process of generating roughness on the surface of the titanium oxide film, which will be described later. Can be appropriately selected.
なお、本発明のＥＰＤのサスペンションに用いられる溶媒としては、ＩＰＡの他に種々の有機溶媒を用いることができ、このような有機溶媒としては、具体的には例えば、アミルベンゼン、イソプロピルベンゼン、エチルベンゼン、キシレン、ジエチルベンゼン、シクロヘキセン、シクロペンタン、ジペンテン、ジメチルナフタレン、シメン類、樟脳油、石油エーテル、石油ベンジン、ソルベントナフサ、デカリン、デカン、テトラリン、テレピン油、灯油、ドデカン、ドデシルベンゼン、トルエン、ナフタレン、ノナン、パインオイル、ピネン、メチルシクロヘキサン、ｐ−メンタン、リグロインといった炭化水素系溶剤を挙げることができる。 As the solvent used for the suspension of EPD of the present invention, various organic solvents can be used in addition to IPA. Specific examples of such organic solvents include amylbenzene, isopropylbenzene, and ethylbenzene. , Xylene, diethylbenzene, cyclohexene, cyclopentane, dipentene, dimethylnaphthalene, cymene, camphor oil, petroleum ether, petroleum benzine, solvent naphtha, decalin, decane, tetralin, turpentine oil, kerosene, dodecane, dodecylbenzene, toluene, naphthalene, Hydrocarbon solvents such as nonane, pine oil, pinene, methylcyclohexane, p-menthane and ligroin can be mentioned.
また、上記有機溶媒としては、アミルアルコール、アリルアルコール、イソアミルアルコール、イソブチルアルコール、ウンデカノール、エタノール、２−エチルブタノール、２−エチルヘキサノール、２−オクタノール、ｎ−オクタノール、グリシドール、シクロヘキサノール、３，５，−ジメチル−１−ヘキシン−３−オール、ｎ−デカノール、テトラヒドロフルフリルアルコール、α−テルピネオール、ネオペンチルアルコール、ノナノール、フーゼル油、ブタノール、フルフリルアルコール、プロパギルアルコール、プロパノール、ヘキサノール、ヘプタノール、ベンジルアルコール、ペンタノール、メタノール、メチルシクロヘキサノール、２−メチル−１−ブタノール、３−メチル−２−ブタノール、３−メチル−１−ブチン−３−オール、４−メチル−２−ペンタノール、３−メチル−１−ペンチン−３−オールといったアルコール類も挙げることができる。 Examples of the organic solvent include amyl alcohol, allyl alcohol, isoamyl alcohol, isobutyl alcohol, undecanol, ethanol, 2-ethylbutanol, 2-ethylhexanol, 2-octanol, n-octanol, glycidol, cyclohexanol, 3, 5 , -Dimethyl-1-hexyn-3-ol, n-decanol, tetrahydrofurfuryl alcohol, α-terpineol, neopentyl alcohol, nonanol, fusel oil, butanol, furfuryl alcohol, propargyl alcohol, propanol, hexanol, heptanol, Benzyl alcohol, pentanol, methanol, methylcyclohexanol, 2-methyl-1-butanol, 3-methyl-2-butanol, 3-methyl-1-butyne - ol, 4-methyl-2-pentanol, 3-methyl-1-pentyn-3-alcohols such ol can also be mentioned.
上記有機溶媒としては、さらにアニソール、エチルイソアミルエーテル、エチル−ｔ−ブチルエーテル、エチルベンジルエーテル、エポキシブタン、クラウンエーテル類、クレジルメチルエーテル、ジイソアミルエーテル、ジイソプロピルエーテル、ジエチルアセタール、ジエチルエーテル、ジオキサン、１，８−シネオール、ジフェニルエーテル、ジブチルエーテル、ジプロピルエーテル、ジベンジルエーテル、ジメチルエーテル、テトラヒドロピラン、テトラヒドロフラン、トリオキサン、ビス（２−クロロエチル）エーテル、フェネトール、ブチルフェニルエーテル、フラン、フルフラール、メチラール、メチル−ｔ−ブチルエーテル、メチルフラン、モノクロロジエチルエーテルといったエーテル・アセタール系溶剤も挙げることができる。 Examples of the organic solvent include anisole, ethyl isoamyl ether, ethyl t-butyl ether, ethyl benzyl ether, epoxy butane, crown ethers, cresyl methyl ether, diisoamyl ether, diisopropyl ether, diethyl acetal, diethyl ether, dioxane, 1,8-cineole, diphenyl ether, dibutyl ether, dipropyl ether, dibenzyl ether, dimethyl ether, tetrahydropyran, tetrahydrofuran, trioxane, bis (2-chloroethyl) ether, phenetole, butylphenyl ether, furan, furfural, methylal, methyl- Mention may also be made of ether-acetal solvents such as t-butyl ether, methylfuran, monochlorodiethyl ether. Kill.
上述の有機溶媒としては、アセチルアセトン、アセトアルデヒド、アセトフェノン、アセトン、イソホロン、エチル−ｎ−ブチルケトン、ジアセトンアルコール、ジイソブチルケトン、ジイソプロピルケトン、ジエチルケトン、シクロヘキサノン、ジ−ｎ−プロピルケトン、ホロン、メシチルオキシド、メチル−ｎ−アミルケトン、メチルイソブチルケトン、メチルエチルケトン、メチルシクロヘキサノン、メチル−ｎ−ブチルケトン、メチル−ｎ−プロピルケトン、メチル−ｎ−ヘキシルケトン、メチル−ｎ−へプチルケトンといったケトン・アルデヒド系溶剤も同様に用いることができる。 Examples of the organic solvent include acetylacetone, acetaldehyde, acetophenone, acetone, isophorone, ethyl-n-butyl ketone, diacetone alcohol, diisobutyl ketone, diisopropyl ketone, diethyl ketone, cyclohexanone, di-n-propyl ketone, phorone, mesityl oxide. Similarly, ketone-aldehyde solvents such as methyl-n-amyl ketone, methyl isobutyl ketone, methyl ethyl ketone, methylcyclohexanone, methyl-n-butyl ketone, methyl-n-propyl ketone, methyl-n-hexyl ketone, and methyl-n-heptyl ketone Can be used.
上述の有機溶媒としては、さらにアジピン酸ジエチル、アジピン酸ジオクチル、アセチルクエン酸トリエチル、アセチルクエン酸トリブチル、アセト酢酸エチル、アセト酢酸アリル、アセト酢酸メチル、アビエチン酸メチル、安息香酸エチル、安息香酸ブチル、安息香酸プロピル、安息香酸ベンジル、安息香酸メチル、イソ吉草酸イソアミル、イソ吉草酸エチル、ギ酸イソアミル、ギ酸イソブチル、ギ酸エチル、ギ酸ブチル、ギ酸プロピル、ギ酸ヘキシル、ギ酸ベンジル、ギ酸メチル、クエン酸トリブチル、ケイ皮酸エステル、ケイ皮酸メチル、ケイ皮酸エチル、酢酸アミル、酢酸アリル、酢酸イソアミル、酢酸イソブチル、酢酸イソプロピル、酢酸エチル、酢酸−２−エチルヘキシル、酢酸シクロヘキシル、酢酸ブチル、酢酸プロピル、酢酸ベンジル、酢酸メチル、酢酸メチルシクロヘキシル、サリチル酸イソアミル、サリチル酸ベンジル、サリチル酸メチル、サリチル酸エチル、蓚酸ジアミル、蓚酸ジエチル、蓚酸ジブチル、酒石酸ジエチル、酒石酸ジブチル、ステアリン酸アミル、ステアリン酸エチル、ステアリン酸ブチル、セパシン酸ジオクチル、セパシン酸ジブチル、炭酸ジエチル、炭酸ジフェニル、炭酸ジメチル、乳酸アミル、乳酸エチル、乳酸メチル、フタル酸ジエチル、フタル酸ジオクチル、フタル酸ジブチル、フタル酸ジメチル、γ−ブチロラクトン、プロピオン酸イソアミル、プロピオン酸エチル、プロピオン酸ブチル、プロピオン酸エチル、プロピオン酸ベンジル、プロピオン酸メチル、ホウ酸エステル類、マレイン酸ジオクチル、マレイン酸ジブチル、マロン酸ジイソプロピル、マロン酸ジエチル、マロン酸ジメチル、酪酸イソアミル、酪酸イソプロピル、酪酸エチル、酪酸ブチル、酪酸メチル、燐酸エステル類といったエステル系溶剤も挙げることができる。 Examples of the organic solvent further include diethyl adipate, dioctyl adipate, triethyl acetyl citrate, tributyl acetyl citrate, ethyl acetoacetate, allyl acetoacetate, methyl acetoacetate, methyl abietic acid, ethyl benzoate, butyl benzoate, Propyl benzoate, benzyl benzoate, methyl benzoate, isoamyl isovalerate, ethyl isovalerate, isoamyl formate, isobutyl formate, ethyl formate, butyl formate, propyl formate, hexyl formate, benzyl formate, methyl formate, tributyl citrate, Cinnamic acid ester, methyl cinnamate, ethyl cinnamate, amyl acetate, allyl acetate, isoamyl acetate, isobutyl acetate, isopropyl acetate, ethyl acetate, 2-ethylhexyl acetate, cyclohexyl acetate, butyl acetate, propyl acetate, vinegar Benzyl, methyl acetate, methyl cyclohexyl acetate, isoamyl salicylate, benzyl salicylate, methyl salicylate, ethyl salicylate, diamyl oxalate, diethyl oxalate, dibutyl oxalate, diethyl tartrate, dibutyl tartrate, amyl stearate, ethyl stearate, butyl stearate, sepacic acid Dioctyl, dibutyl sepacate, diethyl carbonate, diphenyl carbonate, dimethyl carbonate, amyl lactate, ethyl lactate, methyl lactate, diethyl phthalate, dioctyl phthalate, dibutyl phthalate, dimethyl phthalate, γ-butyrolactone, isoamyl propionate, propionic acid Ethyl, butyl propionate, ethyl propionate, benzyl propionate, methyl propionate, borate esters, dioctyl maleate, dibutyl maleate, malo There may also be mentioned ester solvents such as diisopropyl acid, diethyl malonate, dimethyl malonate, isoamyl butyrate, isopropyl butyrate, ethyl butyrate, butyl butyrate, methyl butyrate and phosphates.
上述の溶媒としては、エチレングリコール、エチレングリコールジブチルエーテル、エチレングリコールジアセタート、エチレングリコールジブチルエーテル、エチレングリコールジメチルエーテル、エチレングリコールモノアセタート、エチレングリコールモノイソプロピルエータル、エチレングリコールモノエチルエーテル、エチレングリコールモノエチルエーテルアセタート、エチレングリコールモノフェニルエーテル、エチレングリコールモノブチルエーテル、エチレングリコールモノブチルエーテルアセタート、エチレングリコールモノヘキシルエーテル、エチレングリコールモノメチルエーテル、エチレングリコールモノメチルエーテルアセタート、エチレングリコールモノメトキシメチルエーテル、エチレンクロロヒドリン、１，３−オクチレングリコール、グリセリン、グリセリン１，３−ジアセタート、グリセリンジアルキルエーテル、グリセリン脂肪酸エステル、グリセリントリアセタート、グリセリントリラウラート、グリセリンモノアセタート、２−クロロ−１，３−プロパンジオール、３−クロロ−１，２−プロパンジオール、ジエチレングリコール、ジエチレングリコールエチルメチルエーテル、ポリプロピレングリコールといった多価アルコール及びそれらの誘導体を挙げることができる。 Examples of the solvent include ethylene glycol, ethylene glycol dibutyl ether, ethylene glycol diacetate, ethylene glycol dibutyl ether, ethylene glycol dimethyl ether, ethylene glycol monoacetate, ethylene glycol monoisopropyl ether, ethylene glycol monoethyl ether, ethylene glycol Monoethyl ether acetate, ethylene glycol monophenyl ether, ethylene glycol monobutyl ether, ethylene glycol monobutyl ether acetate, ethylene glycol monohexyl ether, ethylene glycol monomethyl ether, ethylene glycol monomethyl ether acetate, ethylene glycol monomethoxymethyl ether, ethylene Chlorohydrin, , 3-octylene glycol, glycerol, glycerol 1,3-diacetate, glycerol dialkyl ether, glycerol fatty acid ester, glycerol triacetate, glycerol trilaurate, glycerol monoacetate, 2-chloro-1,3-propanediol, Mention may be made of polyhydric alcohols such as 3-chloro-1,2-propanediol, diethylene glycol, diethylene glycol ethyl methyl ether, polypropylene glycol and their derivatives.
さらに上述の溶媒としては、エチルフェノール、オクチルフェノール、カテコール、グアヤコール、キシレノール、ｐ−クミルフェノール、クレゾール、ドデシルフェノール、ナフトール、ノニルフェノール、フェノール、ベンジルフェノール、ｐ−メトキシエチルフェノールといったフェノール類、アセトニトリル、アセトンシアノヒドリン、アニリン、アリルアミン、アミルアミン、イソキノリン、イソブチルアミン、イソプロパノールアミン類、イソプロピルアミン、イミダゾール、Ｎ−エチルエタノールアミン、２−エチルヘキシルアミン、Ｎ−エチルモルホリン、エチレンジアミン、カプロラクタム、キノリン、クロロアニリン、シアノ酢酸エチル、ジアミルアミン、イソブチルアミン、ジイソプロピルアミン、ジイソプロピルエチルアミン、ジアエタノールアミン、Ｎ，Ｎ−ジエチルアニリン、ジエチルアミン、ジエチルベンジルアミン、ジエチレントリアミン、ジオクチルアミン、シクロヘキシルアミン、トリエチルアミン、トリアミルアミン、トリオクチルアミン、トリエタノールアミン、トリエチルアミン、トリオクチルアミン、トリ−ｎ−ブチルアミン、トリプロピルアミン、トリメチルアミン、トルイジン、ニトロアニソール、ピコリン、ピペラジン、ピラジン、ピリジン、ピロリジン、Ｎ−フェニルモルホリン、モルホリン、ブチルアミン、ヘプチルアミン、ルチジンといった含窒素化合物、これらの溶媒の他、含イオウ化合物系溶剤等も挙げることができ、これらの溶剤は、いかなる種類および添加量で混合して用いることができる。その他、ノニオン系、アニオン系、カチオン系および高分子界面活性剤を含む界面活性剤を適宜添加することもできる。 Further, the above-mentioned solvents include ethylphenol, octylphenol, catechol, guaiacol, xylenol, p-cumylphenol, cresol, dodecylphenol, naphthol, nonylphenol, phenols such as phenol, benzylphenol, p-methoxyethylphenol, acetonitrile, acetone Cyanohydrin, aniline, allylamine, amylamine, isoquinoline, isobutylamine, isopropanolamines, isopropylamine, imidazole, N-ethylethanolamine, 2-ethylhexylamine, N-ethylmorpholine, ethylenediamine, caprolactam, quinoline, chloroaniline, ethyl cyanoacetate , Diamylamine, isobutylamine, diisopropylamine, diisopropyl ether Ruamine, diaethanolamine, N, N-diethylaniline, diethylamine, diethylbenzylamine, diethylenetriamine, dioctylamine, cyclohexylamine, triethylamine, triamylamine, trioctylamine, triethanolamine, triethylamine, trioctylamine, tri-n -Nitrogen-containing compounds such as butylamine, tripropylamine, trimethylamine, toluidine, nitroanisole, picoline, piperazine, pyrazine, pyridine, pyrrolidine, N-phenylmorpholine, morpholine, butylamine, heptylamine, lutidine, sulfur solvents other than these solvents Compound solvents and the like can also be mentioned, and these solvents can be mixed and used in any kind and addition amount. In addition, surfactants including nonionic, anionic, cationic, and polymeric surfactants can be added as appropriate.
続いて、上述の手順で調整されたサスペンション１０に紫外線が照射される。紫外線照射には水銀キセノンランプを用いることができる。紫外線照射によって酸化チタン粒子１６にはホール（ｈ＋）と電子（ｅ−）が生じ、ホール（ｈ＋）は、酸化チタン粒子１６の表面に移動したのち、下記反応式にしたがって、ＩＰＡを分解し、アセトンとプロトンを生成する。電子（ｅ−）は、酸化チタン粒子１６の内部にトラップされ、またその一部は、内部の酸化チタンを還元していると考えられる。
Subsequently, the
ここで、カソード電極である、導電体１２の近傍では、酸化チタン膜の形成と同時に、上述した酸化チタンの酸化反応によって生成されたアセトンから、下記の反応式にしたがって、プロパンのガス種の生成が起こる。
Here, in the vicinity of the
上述した手順でＥＰＤが終了したのち、酸化チタン粒子１６によって被覆された導電体１２は、室温で自然乾燥され、本発明の酸化チタン光触媒材料が作製される。また、上記乾燥過程の後、公知の方法で焼成することもできる。
After the EPD is completed by the procedure described above, the
本発明の特定の実施の形態においては、サスペンション１０に、紫外線照射を行う代わりに、サスペンション１０に予めアセトンと水を微量添加することもできる。添加されたアセトンと水由来のＨ＋とが、カソード電極近傍で、反応式（１）にしたがって、上述したのと同様にプロパンのガス種を生成する。しかし、本実施形態においては、水由来のＨ＋が消費された時点でプロパンの生成反応は起こらなくなるため、複数回ＥＰＤを行う場合は、適宜アセトンおよび水をサスペンションに添加して調整することが望ましい。
In a specific embodiment of the present invention, a small amount of acetone and water may be added to the
図２は、本発明の酸化チタン光触媒材料を含む光触媒水浄化装置２０を示す。水槽２２の中に、上述の方法によって作製された多孔質酸化チタン光触媒材料２４が、１枚または２以上の複数枚並べられ、電源２６に接続されてアノード電極として機能する。また、電極２８は、電源２６に接続されてカソード電極として機能する。水槽２２に満たされた被浄化水は、ポンプ３０によって適宜循環される。水槽２２は、紫外線を透過しうる材質でできており、水槽２２の外側近傍に、１本または２以上の複数本のブラックライト３２が配設されている。以下、本発明の光触媒水浄化装置２０の機能について説明する。
FIG. 2 shows a photocatalytic
酸化チタン光触媒材料２４は、ブラックライト３２から紫外線照射を受ける。紫外線の照射により、酸化チタン光触媒材料２４に含まれる酸化チタンにホール（ｈ＋）と電子(
e-)が生じる。この際、酸化チタン光触媒材料２４は、アノード電極として電源２６に接続されているため、バンドの曲がりが生じ、電子（ｅ−）が酸化チタン内部に引っ張られることで、ホール（ｈ＋）が酸化チタン表面への移動が促進され、酸化チタン光触媒材料２４の表面ホール濃度が好適に上昇する。このため、酸化チタン光触媒材料２４の表面触媒活性は向上している。
The titanium
e -) occurs. At this time, since the titanium
また、電源２６によって、電極２８と、酸化チタン光触媒材料２４との間にバイアスをかけることによって、たとえば、電子密度の高い分子を、アノード電極として機能する酸化チタン光触媒材料２４に好適に吸着させることができる。本発明においては、電極２８と、酸化チタン光触媒材料２４との間に設けられる電位差は、上述した表面ホール濃度の上昇と、浄化対象分子の吸着とが好適に起こるように適宜設定することができる。１−４ジオキサンの中間体である、ＥＧＤＦ（エチレングリコールジフォルメイト）は、酸化チタンに吸着性がないため、従来の酸化チタン光触媒では最終分解することができなかったが、ＥＧＤＦは、二重結合を２つ持つ電子密度の高い分子であるため、本発明の光触媒水浄化装置２０における酸化チタン光触媒材料２４には好適に吸着され、上述した表面ホール濃度の高さと相まって、１−４ジオキサンの分解を促進することができる。さらに、本発明によって、同じく電子密度の高い化合物である、ジクロロエタン、トリクロロエタン、２−エチルヘキシルクロリド、塩化アミル、塩化イソプロピル、塩化エチル、塩化ナフタレン、塩化ブチル、塩化ヘキシル、塩化メチル、塩化メチレン、ｏ−クロロトルエン、ｐ−クロロトルエン、クロロベンゼン、四塩化炭素、ジクロロエチレン、ジクロロトルエン、ジクロロブタン、ジクロロプロパン、ジクロロベンゼン、テトラクロロエタン、テトラクロロエチレン、テトラブロモエタン、テトラメチレンクロロブロミド、トリクロロエチレン、トリクロロベンゼン、ブロモクロロエタン、１−ブロモ−３−クロロプロパン、ヘキサクロロエタン、ペンタメチレンクロロブロミド等のハロゲン化炭化水素や、ポリ塩素化ジベンゾパラジオキシン（ＰＣＤＤｓ）及びポリ塩素化ジベンゾフラン（ＰＣＤＦｓ）に代表されるダイオキシン類およびコプラナーＰＣＢについても、分解を促進することができ、各種環境ホルモンなどの芳香族化合物全般の分解を促進することもできる。
In addition, by applying a bias between the
以下、本発明の酸化チタン光触媒材料について実施例を用いてより具体的に説明する。 Hereinafter, the titanium oxide photocatalyst material of the present invention will be described more specifically with reference to examples.
（実施例１）
和光純薬製試薬ＩＰＡ（イソプロピルアルコール、純度９９．５％）１５０ｍｌに対し石原産業株式会社製酸化チタン粉末（ＳＴ−４１：アナターゼ）を３ｇ添加し、６０分撹拌した後、１０分間超音波（BransonUltrasonicsCorp.製 ２５１０Ｊ−ＤＴＨ、４２ｋＨＺ、１００Ｗ）で分散した。さらに、このサスペンションに、撹拌しながら、水銀キセノンランプを用いて１５０ｍＷ／ｃｍ２の強度の紫外線を３０分照射した。次に、このサスペンションに、予め１ＭＮａＯＨで、表面処理した後、蒸留水とアセトンで充分に洗浄した、ＳＵＳ３１６製ステンレスメッシュ（ワイヤー径０．３７５ｍｍ、目開き０．６４ｘ１．０４ｍｍ、Ｐ−タイプ、日本フィルコン社製）をカソードに、予めアセトンで洗浄したアルミニウム板をアノードにし、カソードとアノードとの間隔を１０ｍｍに保持して、ＤＣ電源（高砂株式会社製、ＧＰ０２５０−１）を用い、１９５Ｖの電位でＥＰＤ成膜を３０秒行った。ＥＰＤの後、得られた膜を室温の大気中で１日乾燥したのち、５００℃で３０分焼成した。この際、加熱および冷却は、２℃／分で行った。
Example 1
3 g of titanium oxide powder (ST-41: anatase) manufactured by Ishihara Sangyo Co., Ltd. was added to 150 ml of Wako Pure Chemical Industries IPA (isopropyl alcohol, purity 99.5%) and stirred for 60 minutes, followed by ultrasonication ( 2510J-DTH, 42 kHz, 100 W) manufactured by Branson Ultrasonics Corp. Further, the suspension was irradiated with ultraviolet rays having an intensity of 150 mW / cm 2 for 30 minutes using a mercury xenon lamp while stirring. Next, this suspension was surface treated with 1M NaOH in advance, and then thoroughly washed with distilled water and acetone. A stainless steel mesh made of SUS316 (wire diameter 0.375 mm, aperture 0.64 × 1.04 mm, P-type, Japan (Filcon) was used as the cathode, an aluminum plate previously washed with acetone was used as the anode, the distance between the cathode and anode was maintained at 10 mm, and a DC power source (manufactured by Takasago Co., Ltd., GP0250-1) was used. Then, EPD film formation was performed for 30 seconds. After EPD, the obtained film was dried in air at room temperature for 1 day and then baked at 500 ° C. for 30 minutes. At this time, heating and cooling were performed at 2 ° C./min.
作製された酸化チタン膜の微細構造を、ＳＥＭ（ＪＥＯＬ製、ＪＳＭ−５３１０）によって観察した。その結果、焼成前後でコーティング膜にクラックの発生は見られなかった。また膜表面には多孔質構造が付与された。膜表面の表面粗さ（算術平均粗さＲａ）を、評価したところ、後述する実施例３の場合に比べ、Ｒａが、２０〜３０％増加したことがわかった。図３(ａ)は、多孔質構造が付与された酸化チタン膜表面のＳＥＭ像を示す。 The microstructure of the produced titanium oxide film was observed by SEM (manufactured by JEOL, JSM-5310). As a result, no crack was observed in the coating film before and after firing. The membrane surface was given a porous structure. When the surface roughness (arithmetic average roughness Ra) of the film surface was evaluated, it was found that Ra was increased by 20 to 30% as compared with Example 3 described later. FIG. 3A shows an SEM image of the surface of the titanium oxide film provided with a porous structure.
（実施例２）
実施例１と同様の条件で、ＥＰＤ成膜を、６０秒および１２０秒、それぞれ行い、得られた膜を、実施例１と同様の条件で乾燥・焼成した。図３（ｂ）は、ＥＰＤ成膜を６０秒行った場合の酸化チタン膜のＳＥＭ像を示し、図３（ｃ）は、ＥＰＤ成膜を１２０秒行った場合の酸化チタン膜表面のＳＥＭ像を示す。ＥＰＤの時間を増加させると、表面の粗さが目立たなくなっていった。
(Example 2)
EPD film formation was performed for 60 seconds and 120 seconds under the same conditions as in Example 1, and the obtained film was dried and baked under the same conditions as in Example 1. FIG. 3B shows an SEM image of the titanium oxide film when the EPD film is formed for 60 seconds, and FIG. 3C shows an SEM image of the surface of the titanium oxide film when the EPD film is formed for 120 seconds. Indicates. When the EPD time was increased, the surface roughness became inconspicuous.
（実施例３）
実施例１の紫外線照射の代わりにアセトンをＩＰＡに対して１２７ｐｐｍ外部から添加して作製したサスペンションに対して同様の条件でＥＰＤ成膜を行った。得られた膜を、実施例１と同様の条件で乾燥・焼成した。焼成前後でコーティング膜にクラックの発生は見られなかった。また膜表面には多孔質構造が付与された。図４（ａ）は、実施例３の酸化チタン膜表面のＳＥＭ像を示す。
(Example 3)
EPD film formation was performed under the same conditions on a suspension prepared by adding acetone from the outside by 127 ppm to IPA instead of the ultraviolet irradiation in Example 1. The obtained film was dried and fired under the same conditions as in Example 1. Cracks were not observed in the coating film before and after firing. The membrane surface was given a porous structure. 4A shows an SEM image of the surface of the titanium oxide film of Example 3. FIG.
（比較例１）
実施例３のアセトンの代わりに、水をＩＰＡに対して１２７ｐｐｍ外部から添加して作製したサスペンションに対して、実施例３と同様の条件でＥＰＤ成膜・乾燥・焼成を行った。焼成前後でコーティング膜にクラックの発生は見られなかったが、膜表面には多孔質構造が付与されなかった。図４（ｂ）は、比較例１の酸化チタン膜表面のＳＥＭ像を示す。
(Comparative Example 1)
EPD film formation, drying, and firing were performed under the same conditions as in Example 3 on a suspension prepared by adding 127 ppm of water to IPA from the outside instead of acetone in Example 3. Cracks were not observed in the coating film before and after firing, but no porous structure was imparted to the film surface. FIG. 4B shows an SEM image of the surface of the titanium oxide film of Comparative Example 1.
（比較例２）
和光純薬製試薬ＩＰＡ（イソプロピルアルコール、純度９９．５％）１００ｍｌに対し石原産業株式会社製酸化チタン粉末（ＳＴ−４１）を２ｇ添加し、６０分撹拌した後、１０分間超音波（BransonUltrasonicsCorp.製 ２５１０Ｊ−ＤＴＨ、４２ｋＨＺ、１００Ｗ）で分散した。このサスペンションに、紫外線照射を行うことなく、実施例１と同様の条件でＥＰＤ成膜・乾燥・焼成を行った。焼成前後でコーティング膜にクラックの発生は見られなかったが、膜表面に多孔質構造は付与されなかった。図５は、比較例２の酸化チタン膜表面のＳＥＭ像を示す。
(Comparative Example 2)
2 g of titanium oxide powder (ST-41) manufactured by Ishihara Sangyo Co., Ltd. was added to 100 ml of Wako Pure Chemical Industries IPA (isopropyl alcohol, purity 99.5%) and stirred for 60 minutes, followed by ultrasonication (BransonUltrasonics Corp. Manufactured 2510J-DTH, 42 kHz, 100 W). This suspension was subjected to EPD film formation, drying, and firing under the same conditions as in Example 1 without performing ultraviolet irradiation. Cracks were not observed in the coating film before and after firing, but no porous structure was imparted to the film surface. FIG. 5 shows an SEM image of the surface of the titanium oxide film of Comparative Example 2.
本発明により金属担体を用いた光触媒フィルターの作製手法に新たな可能性を提供できる。またこれを利用して従来、光触媒での分解が困難であった物質を電位等を併用することで効率的に分解するためのシステムが設計できる。本発明により酸化チタン光触媒を用いた効果的な浄化技術が確立できる。 According to the present invention, a new possibility can be provided for a method for producing a photocatalytic filter using a metal carrier. In addition, a system for efficiently decomposing a substance that has been difficult to decompose with a photocatalyst by using a potential or the like can be designed by using this. According to the present invention, an effective purification technique using a titanium oxide photocatalyst can be established.
１０…サスペンション、１２…導電体、１４…電極、１６…酸化チタン粒子、１８…ＤＣ電源、２０…光触媒水浄化装置、２２…水槽、２４…酸化チタン光触媒材料、２６…電源、２８…電極、３０…ポンプ、３２…ブラックライト
DESCRIPTION OF
Claims (15)
前記製造方法は、
溶媒と酸化チタン粉末とからサスペンションを作製する工程と、
前記サスペンションに紫外線を照射する工程と、
前記紫外線を照射されたサスペンション中で電気泳動電着を行い、前記酸化チタン粉末を前記導電性の基体上に堆積させつつガスを発生させる工程と、
を含む製造方法。 A method for producing a photocatalytic material in which a porous titanium oxide film is formed on a conductive substrate,
The manufacturing method includes:
Producing a suspension from a solvent and titanium oxide powder;
Irradiating the suspension with ultraviolet rays;
Performing electrophoretic electrodeposition in the suspension irradiated with the ultraviolet rays, and generating gas while depositing the titanium oxide powder on the conductive substrate;
Manufacturing method.
前記製造方法は、
溶媒と酸化チタン粉末とからサスペンションを作製する工程と、
前記サスペンション中で電気泳動電着を行い、前記酸化チタン粉末を前記導電性の基体上に堆積させつつガスを発生させる工程と、
を含む製造方法。 A method for producing a photocatalytic material in which a porous titanium oxide film is formed on a conductive substrate,
The manufacturing method includes:
Producing a suspension from a solvent and titanium oxide powder;
Performing electrophoretic deposition in the suspension and generating a gas while depositing the titanium oxide powder on the conductive substrate;
Manufacturing method.
請求項７または８のいずれか１項に記載の製造方法。 The solvent is an organic solvent containing isopropyl alcohol and acetone.
The manufacturing method of any one of Claim 7 or 8.
前記電極は前記水槽の内部に配設されており、前記アノード電極は、多孔質酸化チタン膜が形成された導電性材料を含む、
光触媒水浄化装置。 A photocatalytic water purification apparatus comprising a water tank, an ultraviolet ray generating member disposed in the vicinity of the water tank, a power source, and a cathode electrode and an anode electrode connected to the power source,
The electrode is disposed inside the water tank, and the anode electrode includes a conductive material on which a porous titanium oxide film is formed,
Photocatalytic water purification device.
前記方法は、
被浄化水の中に、多孔質酸化チタン膜が形成された導電性材料を含むアノード電極とカソード電極とを配設する工程と、
前記電極間に電位差を設ける工程とを含む、
水浄化方法。 A water purification method using a photocatalytic reaction,
The method
Disposing an anode electrode and a cathode electrode containing a conductive material in which a porous titanium oxide film is formed in the water to be purified;
Providing a potential difference between the electrodes,
Water purification method.
請求項１３に記載の水浄化方法。 The potential difference is a potential difference that increases the surface hole concentration of the porous titanium oxide film of the anode electrode and adsorbs the molecules to be purified contained in the water to be purified on the surface of the porous titanium oxide film.
The water purification method according to claim 13.
請求項１３または１４のいずれか１項に記載の水浄化方法。 The molecule to be purified is selected from the group consisting of 1-4 dioxane, a halogen-containing compound and an aromatic compound.
The water purification method of any one of Claim 13 or 14.
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