JP6404324B2 - 光触媒コーティングを付着させる方法および関連するコーティング、テキスタイル材料および光触媒反応における使用 - Google Patents
光触媒コーティングを付着させる方法および関連するコーティング、テキスタイル材料および光触媒反応における使用 Download PDFInfo
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Description
a)半導体材料のナノ粒子の水性および/またはアルコール性懸濁液を用意するステップと、
b)加水分解されたオルガノシランの水性および/またはアルコール性溶液からなるゾルを用意するステップと、
c)上記懸濁液と上記ゾルを混合し、得られた混合物を被覆対象の支持体に付着させるステップと、次いで
d)乾燥操作を行うステップと
を含む方法を提案することによって上記目標を達成することができる。
29Si−NMR分析は、Bruker DRX400分光計によって室温で行われる。ケイ素29(79.49MHz)の液体NMR測定は、8μsのパルス持続時間を用いて記録される。繰返し時間は5sである。サンプルは、重水素化アセトン(D6)および基準のテトラメチルシラン(TMS)で満たされた1mmのキャピラリーを備えた直径5mmの管内に置かれる。各サンプルについて128回のスキャンが収集された。MestReNovaプログラムが、ハイブリッドゾル−ゲル材料中に存在する様々な化学種の百分率分布を見積るために用いられる。
スペクトルは、4mmのDVTプローブを備えた500MHzのWB Avance III Bruker分光計で記録された。共鳴周波数は、1Hでは500.16MHz、29Siでは99.36MHzである。マジック角回転速度は10kHzである。分析は、300sの緩和時間、200回のスキャン数でプロトンデカップリング(スピンデカップリング80kHz)を用いた直接励起によって行われる。
サンプルは、ボンベ容器(H2SO4+HNO3+HF)における酸攻撃および150℃オーブンでの12時間の加熱によって溶液にされる。TiおよびSi元素の定量は、ICP−OES(誘導結合プラズマ−発光分光分析)によって達成される。分析は、Jobin Yvonブランドの「Activa」装置で行われる。この装置によって、160nm〜800nmのスペクトル範囲をカバーできる。
SEM顕微鏡写真は、SDD Bruker検出器を備えたFEI Quanta250FEG装置で撮影される。操作パラメータは次の通りであった。
・加速電圧:15kV
・操作距離:4〜7mm
・倍率:×30,000〜×100,000
高圧液相クロマトグラフィー装置は、VarianProstar Model410ポンプと、210nmに調整されたフォトダイオードアレイUVVarianProstar330PDAを有する検出器とを備える。分子を分離するために用いた方法は、有機酸とアルコールを分離するのに有効なH+陽イオン交換カラム(Sarasep CAR−H 7.8mm×300mm)を使用したイオンクロマトグラフィーである。移動相として用いた溶離液は、流量0.7ml/minとした5×10−3M H2SO4である。サンプルの注入量は20μlである。
Bio−link、Fisher Scientific、W×D×H=260×330×145mm。
多孔度は、液体窒素温度(77K)での窒素の吸着/脱着によって調べられる。窒素吸脱着等温線は、Micromeritics ASAP2010装置により得られる。分析前に、サンプルは350℃の温度で7時間真空中で脱気される。
0.83gの市販ナノ粒子(P−25Degussa、70/30〜80/20の間の比率のアナターゼ/ルチル結晶形、25〜35nmの間のサイズ)と0.62mlの酢酸を混合することによって二酸化チタン(TiO2)のスラリーを調製する。次いで、得られたスラリーは、1分間の超音波処理によって6.7mlのエタノール中に分散させる。
フラスコ中で、pH=3.5(HCl)の14モルの酸性水を1モルのCH3−Si(O−CH2−CH3)3前駆体に加える。溶液を17時間撹拌したままにする。次いで、生成したアルコールを135℃での共沸蒸留によって除去する。最後に残った少量の液体は、回転エバポレータを用いて真空蒸留によって除去する。溶液にエーテルを加えることによってゾルから液体を分離する。下層の水性相を除去する。残留する痕跡量のHClを除去するために水による数回の洗滌を行う。最後に残った水分子を除去するためにMgSO4を投入する。最終溶媒であるエタノールを加え、回転エバポレータを用いてエーテルを除去する。所望の乾燥抽出物比率に応じてエタノールを再び加える。
膜(ハイブリッドシリカゾルによる膜)の有機基の濃度は、有機物を含まないシリカゾルを様々な量で添加することによって調節される。このゾルは、前駆体Si(O−CH2−CH3)4の酸加水分解によって合成される。その乾燥抽出物比率は18%、その縮合度は80%である。
SiO2/TiO2質量比を変化させるために、最終溶液中のSiO2およびTiO2ナノ粒子の質量%を利用する。
CH3−Si(O−CH2−CH3)3前駆体の酸加水分解によって合成された縮合度62%のハイブリッドシリカゾルが、縮合度88%のものの代わりに使用される。このために、1モルのCH3−Si(O−CH2−CH3)3前駆体、3モルの酸性水(pH=2.5、HCl)および3モルのエタノールを激しく攪拌しながら加える。この溶液を17時間撹拌したままにした後、冷凍庫に保管する。得られたゾルの乾燥抽出物比率は20%である。膜を調製するための残りの手順は、実施例1と同じままである。図6は、実施例4で得られたコーティングの表面の走査電子顕微鏡画像(SEM)である。この画像は、ランダムな形状およびサイズ(20〜400nmの間の細孔径)の細孔を有するマクロ多孔質およびメソ多孔質を示す。
ビニル型およびプロピル型の有機基を含む他のシリカゾルが試験された。
TiO2ナノ粒子が、ZnO(Sigma−Aldrich、サイズ<100nm)に置き換えられる。膜を調製する残りの手順は、実施例1と同じである。
実施例1で得られた結果が、無機バインダーSiO2を使用してTiO2(PC500、Millennium、アナターゼ≧99%、5〜10nmの間のサイズ)とゼオライトでコーティングされた繊維からなる光触媒紙(Ahlstromにより販売、ref.1048)と比較される。
合成手順は実施例1と同じである。溶液は、以下の2つの異なるテキスタイル支持体に付着された:ポリエチレン(PE)の不織布、および、ポリウレタン(PU)ワニスでコーティングされたポリエチレンテレフタレートの織布。
Claims (16)
- ケイ素原子の17〜97モル%がSi−C結合を介して少なくとも1つの有機基に結合しているポリシロキサンからなるコーティングであって、該コーティング中に半導体材料のナノ粒子が分布しており、該コーティングが多孔質であり、マクロ多孔質を有することを特徴とするコーティング。
- 上記コーティングが水性溶液に浸漬された場合に照明が行われても、上記コーティング中に存在する、Si−C結合を介してケイ素原子に結合した有機基の除去が全く起こらないことを特徴とする、請求項1に記載のコーティング。
- 上記コーティング中に存在する、Si−C結合を介してケイ素原子に結合した有機基の除去が全く起こらない照明が、365nmおよび312nmでそれぞれ光強度を10mW/cm2および3mW/cm2として22℃で6時間行われることを特徴とする、請求項2に記載のコーティング。
- 上記コーティング中に存在する80〜95モル%のケイ素原子が、炭素原子に結合していることを特徴とする、請求項1〜3のいずれか一項に記載のコーティング。
- Si−C結合を介してケイ素原子に結合した有機基が、アルキル基;アリル基;および、ビニル基から選択されることを特徴とする、請求項1〜4のいずれか一項に記載のコーティング。
- 1〜90質量%の半導体材料を含むことを特徴とする、請求項1〜5のいずれか一項に記載のコーティング。
- 上記半導体材料のナノ粒子が、5〜100nmの範囲に属するサイズを有することを特徴とする、請求項1〜6のいずれか一項に記載のコーティング。
- 上記半導体材料のナノ粒子が、TiO2、ZnO、SnO2、WO3、Fe2O3、Bi2O3、SrTiO3、CdS、SiCまたはCeO2のナノ粒子またはそれらナノ粒子の混合物であることを特徴とする、請求項1〜7のいずれか一項に記載のコーティング。
- 上記半導体材料のナノ粒子が、TiO2、ZnO、SnO2、WO3、Fe2O3、Bi2O3、SrTiO3、CdSのナノ粒子またはそれらナノ粒子の混合物であり、Si原子/半導体材料のナノ粒子の金属原子の比が、0.3/1〜5/1の範囲に属すことを特徴とする、請求項1〜8のいずれか一項に記載のコーティング。
- 可撓性であることを特徴とする、請求項1〜9のいずれか一項に記載のコーティング。
- 表面粗さを有することを特徴とする、請求項1〜10のいずれか一項に記載のコーティング。
- 少なくとも90質量%が、ケイ素原子の17〜97モル%がSi−C結合を介して有機基に結合しているポリシロキサンマトリックスおよび半導体材料のナノ粒子からなることを特徴とする、請求項1〜11のいずれか一項に記載のコーティング。
- 請求項1〜12のいずれか一項に記載のコーティングにより被覆されたテキスタイル材料。
- 支持体とコーティングの間の結合が、Si−O結合を介して達成される、請求項1〜12のいずれか一項に記載のコーティングにより被覆された支持体。
- テキスタイルに相当する、請求項14に記載の支持体。
- 有機化合物の光触媒分解のための、請求項1〜12のいずれか一項に記載のコーティング、請求項13に記載のテキスタイル材料または請求項14もしくは15に記載の支持体の使用。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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FR1353122A FR3004130B1 (fr) | 2013-04-08 | 2013-04-08 | Procede de depot d'un revetement photocatalytique, revetements, materiaux textiles et utilisation en photocatalyse associes |
FR1353122 | 2013-04-08 | ||
PCT/FR2014/050822 WO2014167231A2 (fr) | 2013-04-08 | 2014-04-07 | Procédé de dépôt d'un revêtement photocatalytique, revêtements, matériaux textiles et utilisation en photocatalyse associes |
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US (1) | US20160040353A1 (ja) |
EP (1) | EP2983837A2 (ja) |
JP (1) | JP6404324B2 (ja) |
CN (1) | CN105102138A (ja) |
CA (1) | CA2907818A1 (ja) |
FR (1) | FR3004130B1 (ja) |
WO (1) | WO2014167231A2 (ja) |
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KR101989380B1 (ko) * | 2017-02-16 | 2019-06-14 | 한국원자력연구원 | 방사성 세슘 흡착제 및 이를 이용한 방사성 세슘 및 유기오염물질 제거방법 |
KR102160108B1 (ko) * | 2017-12-28 | 2020-09-25 | 한국원자력연구원 | 방사성 세슘 흡착제 및 이를 이용한 방사성 세슘의 제거방법 |
CN115536286B (zh) * | 2022-06-29 | 2024-04-26 | 北京科技大学 | TiO2和SiO2复合纳米涂层、制备及应用 |
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US5616532A (en) * | 1990-12-14 | 1997-04-01 | E. Heller & Company | Photocatalyst-binder compositions |
US5849200A (en) * | 1993-10-26 | 1998-12-15 | E. Heller & Company | Photocatalyst-binder compositions |
CN1081490C (zh) * | 1995-06-19 | 2002-03-27 | 日本曹达株式会社 | 载有光催化剂的构件和光催化剂涂敷材料 |
JP3182107B2 (ja) * | 1996-12-13 | 2001-07-03 | 松下電工株式会社 | 機能性塗装品とその製造方法および用途 |
FR2779751B1 (fr) * | 1998-06-10 | 2003-11-14 | Saint Gobain Isover | Substrat a revetement photocatalytique |
JP2006116449A (ja) * | 2004-10-22 | 2006-05-11 | Asahi Kasei Chemicals Corp | 光触媒繊維、それから誘導される多孔性光触媒繊維 |
US20070141320A1 (en) | 2005-12-21 | 2007-06-21 | Shulong Li | Substrate having photocatalytic and activated carbon constituents and process for producing |
JP2010513587A (ja) * | 2006-12-13 | 2010-04-30 | シレクス オサケユキチュア | 新規ナノ粒子含有シロキサン重合体 |
US8883084B2 (en) * | 2007-07-31 | 2014-11-11 | Carrier Corporation | Siloxane removal via silicate formation for lifetime extension of photocatalytic devices |
US20100130348A1 (en) * | 2007-09-21 | 2010-05-27 | Chul-Hyun Kang | Photocatalytic composition for anti-reflection and the glass substrate coated with the composition |
TW200920796A (en) * | 2007-11-12 | 2009-05-16 | Onid Technology Corp | Transparent aqueous nanometer sol-gel paint composition without reducing visible light and sunlight transmittance of transparent substrates and coating method thereof |
FR2923500B1 (fr) | 2007-11-14 | 2009-11-27 | Porcher Ind | Element souple et ignifuge pourvu d'un revetement photocatalytique, et son procede de fabrication. |
FR2928379B1 (fr) | 2008-03-06 | 2010-06-25 | Centre Nat Rech Scient | Fibres textiles ayant des proprietes photocatalytiques de degradation d'agents chimiques ou biologiques, procede de preparation et utilisation a la photocatalyse |
WO2010001056A2 (fr) | 2008-07-02 | 2010-01-07 | Bluestar Silicones France Sas | Substrat elastomere silicone revetu d'un film anti-salissures contenant un promoteur de photocatalyse et support comprenant un substrat ainsi revetu |
FR2934283B1 (fr) | 2008-07-22 | 2010-09-24 | Ahlstroem Oy | Dalle acoustique perforee depolluante |
JP2010036135A (ja) * | 2008-08-06 | 2010-02-18 | Nitto Denko Corp | 多孔質光触媒皮膜および多孔質光触媒皮膜の製造方法 |
CN101413212B (zh) * | 2008-11-27 | 2011-03-16 | 东华大学 | 一种光催化涂层空气自净化功能织物的制备方法 |
CN101518730B (zh) * | 2009-04-01 | 2011-01-05 | 宇星科技发展(深圳)有限公司 | 一种复合纳米二氧化钛光催化材料及制备方法 |
WO2012069672A1 (es) * | 2010-11-25 | 2012-05-31 | Fundacion Tecnalia Research & Innovation | Recubrimientos fotocatalíticos híbridos, procedimiento para aplicarlos sobre distintos sustratos y usos de los sustratos así recubiertos |
JP2012193523A (ja) * | 2011-03-15 | 2012-10-11 | Ohara Inc | 建材及びその製造方法 |
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CA2907818A1 (fr) | 2014-10-16 |
WO2014167231A3 (fr) | 2014-12-11 |
US20160040353A1 (en) | 2016-02-11 |
FR3004130A1 (fr) | 2014-10-10 |
EP2983837A2 (fr) | 2016-02-17 |
JP2016523688A (ja) | 2016-08-12 |
WO2014167231A4 (fr) | 2015-02-05 |
CN105102138A (zh) | 2015-11-25 |
WO2014167231A2 (fr) | 2014-10-16 |
FR3004130B1 (fr) | 2015-12-11 |
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