JP6830446B2 - 光触媒コーティング - Google Patents
光触媒コーティング Download PDFInfo
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- JP6830446B2 JP6830446B2 JP2017562088A JP2017562088A JP6830446B2 JP 6830446 B2 JP6830446 B2 JP 6830446B2 JP 2017562088 A JP2017562088 A JP 2017562088A JP 2017562088 A JP2017562088 A JP 2017562088A JP 6830446 B2 JP6830446 B2 JP 6830446B2
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- photocatalyst
- photocatalytic
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- dispersion
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Description
1TMA+10.5O2 −> 3CO2+4.5H2O+0.5N2(g)
それゆえに、TMA含有ガス混合物を光触媒材料に接触させ、材料を青色光、例えば約455nmに曝露した後の混合物中におけるCO2の出現は、TMAから成分ガス/組成物への光触媒的な分解を示し得る。
別様に示されない限り、全ての材料はさらなる精製なしに用いた。別様に示されない限り、全ての材料はシグマ・アルドリッチ(セントルイス、MO、USA)から購入した。
2013年1月13日出願の米国特許出願番号13/738,243(2013年7月18日公開の米国特許出願公開2013/0180,932として公開)に記載されている方法に従って調製されたWO3光触媒(200mg)を水に追加した。それから、もたらされた分散液をCeO2ゾル(ニッサンケミカルナノユースCE−20B)の740mgに追加した。CeO2およびWO3のモル比は1:1(50モル%対50モル%)となるように選んだ。それから、水中に約20wt%固体材料であるコーティング溶液を作るために、RO(逆浸透処理)水の十分量(800mg)をもたらされた分散液に追加した。もたらされた分散液を、超音波ホモジナイザーを用いてホモジナイズした。スピンコーター(1200rpm/40sec)を用いることによって、ガラス基材(50mm×75mm)を調製された結果物によってコーティングした。コーティングされた基材を約120℃で約2分間加熱した。もたらされたコーティングされた基材は透明であった(約555nmにおいて約86%)。青色発光ダイオード(LED)(455nm、200mW/cm2)照射の1時間の後の約81%までのアセトアルデヒド分解比率をモニターすることによって、光触媒活性を決定した。
コーティングされた基材2を例1と同様の様式で作った。ただし、SiO2ゾル(ニッサンケミカルSNOWTEX−O、258mg)をCeO2ゾルの代わりに追加した。もたらされたコーティングされた基材は透明であった(約555nmにおいて90%)。アセトアルデヒド分解比率によって決定される光触媒活性は例1と同様の条件下で照射後に約50%であった。
コーティングされた基材3を例1と同様の様式で作った。ただし、SiO2ゾル(ニッサンケミカルSNOWTEX−20L、258mg)をCeO2ゾルの代わりに追加した。もたらされた得られた基材は透明であった(555nmにおいて91%)。アセトアルデヒド分解比率によって決定される光触媒活性は例1と同様の条件下で照射後に約67%であった。
比較例1は例1と同様の様式で調製した。ただし、シリコーン樹脂(信越化学、SCR−1012)をCeO2ゾルの代わりに用いた。WO3の比率はシリコーン樹脂中に約20wt%であった。ガラス基材(50mm×75mm)を調製された溶液によってドクターブレードでコーティングした。硬化のための120℃加熱後に、得られた基材は半透明であった。もたらされた得られた基材は555nmにおいて約75%の透明度を見せた。アセトアルデヒド分解比率によって決定された光触媒活性は例1と同様の条件下で照射後に約1%であった。
比較例2は例1と同様の様式で調製した。ただし、ポリ(メチルメタクリレート)(PMMA)をアセトン中に分散した。WO3の比率はPMMA中に約20wt%であり、水は追加しなかった。ガラス基材(50mm×75mm)を調製された溶液によってドクターブレードでコーティングした。硬化のための120℃加熱後に、得られた基材は半透明であった。もたらされた得られた基材は555nmにおいて約78%の透明度を見せた。アセトアルデヒド分解比率は例1と同様の条件下で照射後に0.5%であった。
WO3(0.8g)をAl2O3ゾル(ニッサンケミカルアルミナゾル200、5g)に追加した。Al2O3およびWO3のモル比は、重量で1:1となるように選ばれた。それから、水中に14wt%固体材料であるコーティング溶液を作るために、RO水(5.8g)を追加した。ガラス基材(50mm×75mm)を、調製された溶液によってスピンコーター(1200rpm/40sec)を用いることによってコーティングした。液体の蒸発のための約120℃における加熱後に、得られた基材は半透明であった。もたらされた得られた基材は透明であった(555nmにおいて91%)。アセトアルデヒド分解比率は例1と同様の条件下で照射後に約0%であった。
5mMタングステン酸(WO3・H2O)の30mLおよびHF2%溶液の30mL(例えばWO3前駆体)をホウ酸(H3BO3)の40mlに追加した。2つの75mm×25mmシリコンウエハをもたらされた溶液中に浸漬し、約30℃で約6時間撹拌した。重層した基材を溶液から取り出し、約400℃で約1時間アニールし、コーティングされたガラススライドをもたらした(例4)。コーティング溶液を十分なCeO2ゾル(ニッサンケミカルナノユースCE−20B)によって調製して、約1:1というCeO2およびWO3のモル比(50モル%対50モル%)を達成した。それから、例1に記載されているものと同様の様式で、上で論じられているようにCeO2コーティング溶液によって例4の基材をスピンコーティングすることによって、例4aを作った。
WO3(グローバル・タングステン&パウダー、トウォンダ、PA、USA[GTP])の5gを、直径が約3mmのZrO2ボールの約50gを含有する高純度アルミナボールミルジャーに追加し、ボールミル(SFM−1モデル卓上遊星ボールミル(MTI−Corp.所在地)によって25mLメタノール中で約4時間粉砕して、より小さい粒径を有する粉砕WO3(GTP)を得た。プラズマWO3は、その全体として参照によってここに組み込まれる米国特許8,003,563に記載されているものと同様の様式で作った。
別の例(例8)においては、追加のスライドを例1のものと同様の様式で作った。ただし、追加されるCeO2ゾルの量を変えて、WO3:CeO2の異なるモル比を達成した(例えば0%、0.1%、5%、10%、30%、50%、75%、90%、95%、100%)((100−x)WO3+(x)Tバインダー)。図5は、270mW/cm2青色LEDアレイ光への曝露の1時間の後に見積もられたアセトアルデヒド分解を示している。
別の例(例9)においては、追加のスライドを次の様式で作った。プラズマWO3粉末(130mg)およびCeO2粉末(96.5mg)(約1:1モル比)を第1にRO水中に分散し(固体の20wt%)、約10分間バスソニケーションし(VWR−B3500A−MT)、それから約5分間プローブソニケーションした(ソニックディスメンブレータモデル100、連続モード)。それから、混合物/複合材料/ブレンドを75mm×50mmガラススライド上にスピンコーティングし、例4に記載されているようにアニールした。
追加のスライドを同様の様式で作った。ただし、表1に示されているように、種々の他の材料をCeO2の代わりに用いた。
加えて、別の例においては、種々の化合物(表2参照)からの粉末化試料の約130mgをそれぞれ別個にRO水の最小限の量に溶解し、約5分間ホモジナイズした。それから、例1に記載されているプロセスに従って、化合物を1:1モル比でWO3と組み合わせた。
別の例においては、またオクチル酸スズ(II)および/またはオクチル酸第一スズ]とし公知の2−エチルヘキサン酸スズ(II)(Spectrum−Chemicals、ガーデナ、CA、USA)の3.78g、Ce(NO3)3・6H20(シグマ・アルドリッチ、セントルイス、MO、USA)の5g、および硝酸アンモニウム(NH4NO3)(シグマ・アルドリッチ、セントルイス、MO、USA)の3.0gをRO処理水の約25mL中に溶解した。それから、混合物を約150℃で加熱し約20分間撹拌するすぐ前に、1.129gマレイン酸ヒドラジドを追加した。
別の例においては、例1に記載されているものと同様の様式でTi(O,C,N)2:SnをプラズマCeO2粉末と組み合わせた(1:1モル比)。ただし、Ti(O,C,N)2:Sn粉末をWO3粉末の代わりに用い、例1に記載されているようにガラスマイクロスライド上にスピンコーティングした。Ti(O,C,N)2:Snを、その全体として参照によってここに組み込まれる2012年3月8日出願の同時係属の米国特許仮出願番号61/608,754に記載されているように、水溶液燃焼法によって、チタン(IV)ビスアンモニウムラクテート二水酸化物(50wt%水溶液の7mL)、オクチル酸スズ(0.883g)、および硝酸アンモニウム(3.5g)に加えて完全に分解可能な燃料としてグリシン(1.4g)を使用して、300℃において合成し、次にボックス炉内において400℃で30分間アニールをした。以前の例のものと同様の様式で作られたガラススライドを、また先に例4に記載されているように(270mW/cm2光強度で)アセトアルデヒド分解について試験した。Tedlarバッグ中のTi(O,C,N)2:Sn光触媒コーティングされたガラススライドについて、曝露の5時間の後に7%のアセトアルデヒド分解が観察された。Ti(O,C,N)2:SnおよびCeO2(1:1モル比)両方を有するガラススライドを同様の様式でTedlarバッグ中において試験したときには、アセトアルデヒド分解は曝露の5時間の後に22%まで増大した。
WO3調製
WO3(Nanostructured&AmorphousマテリアルズInc[NA]、ヒューストン、TX、USA)の5gを、直径が約3mmのZrO2ボールの約50gを含有する高純度アルミナボールミルジャーに追加し、より小さい粒径を有する粉砕WO3(NA)を得るためにボールミル(SFM−1モデル卓上遊星ボールミル[MTI−Corp、リッチモンド、CA、USA])によって25mLメタノール中で約18時間粉砕し、それから約400℃で約5時間アニールした。
例37
加工したNAのWO3の65mgを、216mgのコロイド状ZrO2(ZR−30BF、ニッサンケミカル)および(ミリQ(EMDミリポア、ビレリカ、MA、USA)水から370μlポアフィルターを通過した超精製水の369mgと一緒に20mlガラスバイアルに追加した。NAのWO3対ZrO2のモル比は約1モルのNAのWO3(34.7%)対約1.88モルZrO2(65.3%)であった。コロイド状ZrO2の固体含量は30wt%であった。総分散液WO3/ZrO2の固体含量は20wt%であった。混合物を、第1にソニケーションバス中に5分間置くことによって分散した。懸濁液をソニケーションプローブによって10分間混合することによって、光触媒組成物懸濁液(WO3)の一様なコーティングを得た。
比較例4は例37と同様の様式で調製した。加工したWO3の43mg、CeO2(Richest)の43mg、およびゼオライト(シグマ・アルドリッチ)の43mgを追加した。
例37〜38および比較例3は表4にまとめられている。
それから、それぞれのペトリ皿を真空下で別個の5LのTedlarバッグ中に封入し、次に周囲空気の約3Lおよび2000ppmトリメチルアミンの約150mLを暗環境下で注入した。トリメチルアミン濃度を時間0Hおよび2Hにおいて検知管(ガステック)によって見積もった。ZrO2を含有する例37および38は暗条件下でトリメチルアミンを吸着した(それぞれ約63ppmおよび約72ppm)。ZrO2の代わりにゼオライトを含有する比較例4は暗条件下でトリメチルアミンのより少ない量を吸着した(約50ppm)。ZrO2もいずれかのWO3も含有しないブランクフィルターは、暗条件下でいかなるトリメチルアミン(約50ppm)も明らかには吸着しなかった。これらの結果は表5にまとめられている。
加工したWO3の2000mg、CeO2の1485mg、およびZrO2ゾルの1773mg(ZR−30BF。固体ZrO2の532mgを含有する)を精製水の14827mgに追加した(1:1:0.5モル比組成物)。
工場は一般照明のための有機発光ダイオード照明設備を備える。この環境光は樹脂表面と反応し得、それによって表面に酸素ラジカルを作り出す。それらのラジカルは食品コンタミナントと反応し得、それによって食品を安全にする。樹脂を作業表面に適用する結果として、細菌が食品供給中に広がる事例は50%低下した。
同じ冷蔵庫システム内に置かれた同じフィルター処理素子/フィルター処理システムを以前の試験から約2時間後に繰り返して、システムの連続的な有効性を評価した。結果は図11に示されている。
試料調製(フィルターNo.1からフィルターNo.5)
加工したWO3の2000mg、CeO2の1485mg、およびZrO2ゾルの5670mg(ZR−30BF。固体ZrO2の1701mgを含有する)を精製水の16775mgに追加した(1:1:1.6モル比組成物)。
さらに、フィルターNo.2をフィルターNo.3と同じ様式で調製した。ただし、光触媒組成物はZrO2ゾルを用いることなしに調製した。
さらにその上に、ACフィルター(活性炭)をフィルターNo.5として用いた。
酢(中国の市販製品)の0.11gを濾紙に包含し、アクリルボックス中に配置されたペトリ皿上に置いた。評価は、パーソナルTVOCモニターFTVR−01(フィガロ、日本国)を用いて行った。結果は下の表7にNo.1として示した。
さらに、上述のNo.1と同様の評価を、フィルターNo.1の代わりにフィルターNo.2を用いることによって行った。結果を下の表7にNo.2として示した。
さらに、上述のNo.1と同様の評価を、フィルターNo.1の代わりにフィルターNo.3を用いることによって行った。結果を下の表7にNo.3として示した。
さらに、上述のNo.1と同様の評価を、フィルターを用いないことによって行った。結果を下の表7にNo.4として示した。
さらに、上述のNo.1と同様の評価を、フィルターNo.1の代わりにフィルターNo.5を用いることによって行った。結果を下の表7にNo.5として示した。
その上、これらの評価結果は図12にもまた示されている。
Claims (18)
- WO3を含む光触媒と、
ZrO2、活性炭、およびAl2O3の少なくとも1つを含む吸着剤材料と、
CeO2を含む助触媒と、
を含む光触媒組成物であって、
前記光触媒および/または前記助触媒の含有量と、前記吸着剤材料の含有量のモル比が、1:0.25〜1:5である光触媒組成物。 - 前記光触媒が少なくとも1つの天然に存在する元素をドープされている、
請求項1に記載の光触媒組成物。 - 前記光触媒が遷移金属、遷移金属酸化物、または遷移金属水酸化物を担持する、
請求項1又は2に記載の光触媒組成物。 - 前記遷移金属がCu、Fe、またはNiである、
請求項3に記載の光触媒組成物。 - 前記光触媒が貴金属、貴金属酸化物、または貴金属水酸化物を担持する、
請求項1〜4のいずれか一項に記載の光触媒組成物。 - 前記貴金属がAu、Ag、Pt、Pd、Ir、Ru、またはRhである、
請求項5に記載の光触媒組成物。 - 前記光触媒組成物がトリメチルアミンを光触媒的に分解する能力がある、
請求項1〜6のいずれか一項に記載の光触媒組成物。 - 請求項1〜7のいずれか一項に記載の光触媒組成物を含む、光触媒層。
- さらに基材を含み、
前記光触媒組成物の少なくとも一部分が前記基材表面に接触する、
請求項8に記載の光触媒層。 - 前記光触媒組成物または前記光触媒層が塩基性ガスおよび/または酸性ガスを除去するために用いられる、
請求項1〜7のいずれか一項に記載の光触媒組成物または請求項8もしくは9に記載の光触媒層の使用。 - 前記塩基性ガスがトリメチルアミンを含む、
請求項10に記載の使用。 - 前記酸性ガスが酢酸を含む、
請求項10に記載の使用。 - 請求項1〜7のいずれか一項に記載の光触媒組成物を形成することと、前記光触媒組成物を基材に適用することとを含む、
光触媒層の製造方法。 - WO3を含む光触媒と、
ZrO2、活性炭、およびAl2O3の少なくとも1つを含む吸着剤と、
CeO2を含む助触媒と、
を含む光触媒層の製造方法であって、
前記光触媒と前記吸着剤とCeO2と分散媒とを含む分散液を生成することにおいて、前記光触媒と前記CeO2と前記吸着剤のモル分率が、20〜50モル%の光触媒、20〜50%のCeO2、及び5〜60モル%の吸着剤材料であることと、
前記分散液を基材に適用することと、
前記分散液から実質的に全ての前記分散媒を蒸発させるために十分な温度および時間の長さで前記分散液および前記基材を加熱することと、
を含む、製造方法。 - 前記光触媒と前記CeO2と前記吸着剤とのモル比が、1:1:0.25から1:1:2である、
請求項14に記載の製造方法。 - 請求項1〜7のいずれか一項に記載の光触媒組成物を含む、セルフクリーニング材料。
- 前記光触媒組成物がガラス、壁板、石材、石造建築物、金属、木材、プラスチック、コンクリート、繊維、布、糸、またはセラミックに適用される、
請求項13に記載の方法。 - 前記光触媒組成物が蒸着、化学蒸着、物理蒸着、ラミネーション、プレス処理、ローラー処理、ソーキング、溶融、糊付、ゾル−ゲル成膜、スピンコーティング、ディップコーティング、バーコーティング、ブラシコーティング、スパッタリング、溶射、フレーム溶射、プラズマ溶射、高速酸素−燃料溶射、原子層堆積、コールドスプレー、またはエアロゾルデポジションによって適用される、
請求項13に記載の方法。
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