JP4862183B2 - 光触媒用酸化チタンの製造方法及びチタニア/有機複合体の製造方法 - Google Patents
光触媒用酸化チタンの製造方法及びチタニア/有機複合体の製造方法 Download PDFInfo
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- JP4862183B2 JP4862183B2 JP2006065671A JP2006065671A JP4862183B2 JP 4862183 B2 JP4862183 B2 JP 4862183B2 JP 2006065671 A JP2006065671 A JP 2006065671A JP 2006065671 A JP2006065671 A JP 2006065671A JP 4862183 B2 JP4862183 B2 JP 4862183B2
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- titanium oxide
- titania
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 179
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 68
- 239000011941 photocatalyst Substances 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000002131 composite material Substances 0.000 title claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 66
- 229910052757 nitrogen Inorganic materials 0.000 claims description 33
- 230000001699 photocatalysis Effects 0.000 claims description 21
- -1 titanium alkoxide Chemical class 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 229910052719 titanium Inorganic materials 0.000 claims description 19
- 239000010936 titanium Substances 0.000 claims description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 125000004432 carbon atom Chemical group C* 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
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- 125000000217 alkyl group Chemical group 0.000 claims description 12
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- 239000001301 oxygen Substances 0.000 claims description 12
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- 239000011261 inert gas Substances 0.000 claims description 11
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- 125000003118 aryl group Chemical group 0.000 claims description 8
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
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- 239000005711 Benzoic acid Substances 0.000 description 2
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 2
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- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
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- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
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Images
Description
具体的なチタンアルコキシドとしてはチタンエトキシド、チタンメトキシド、チタンイソプロポキシド、チタン−n−ブトキシド等が挙げられる。
窒素雰囲気下、チタンテトライソプロポキシド(50mmol)とイソステアリン酸(25mmol)を混合し、o−キシレンにて全量60mLに希釈した。一方、イソステアリン酸(5mmol)とn−ヘキシルアミン(5mmol)を混合し、o−キシレンにて全量40mLに希釈して重縮合を促進させるための塩触媒溶液とした。両者を混合後、上部に二つの小孔をあけた容器に入れ、一方の小孔から10℃で水分を飽和させた加湿窒素を流通させ、反応容器を40℃に保持したまま溶液をかくはんし、反応を進行させた。このような反応条件では反応容器内の相対湿度が約17%に保持される。以上のような反応を4日間行い、チタニア/イソステアレート複合体からなるゾルを得た。
実施例1のチタニア/アンモニウム複合体の合成の際に必要な水分導入を、空気中の水分を徐々に取り込むことによって行った。その余は実施例1と同様とした。XRDを測定したところ、実施例1とほとんど同様なアナターゼ酸化チタンに帰属されるピークのみが観察され、両者の結晶性に大きな差異は認められなかった。得られた酸化チタンには可視光域の強い吸収が観察される一方、比表面積は8m2g-1と小さく、可視光照射下での光触媒能は実施例1に比較して低かった(図2参照)。
実施例1における加熱処理時に流通させる混合ガスの酸素の濃度を0%(窒素100%)とした。その余は実施例1と同様とした。XRDを測定したところ、アナターゼ酸化チタンに帰属されるピークのみが観察され、アナターゼ結晶型の酸化チタンであることが確認できた。得られた酸化チタンの比表面積は167m2g-1であった。実施例1と同様可視光照射下での光触媒能を評価したところ、図2に示すように、顕著な分解が観察され、高い光触媒能を示した。ドープされた窒素量は約0.05重量%であった。
実施例2における加熱処理時に流通させる混合ガスの酸素の濃度を20%とした。その余は実施例2と同様とした(実施例1に同じ)。XRDを測定したところ、実施例2とほとんど同様なアナターゼ酸化チタンに帰属されるピークのみが観察され、両者の結晶性に大きな差異は認められなかった。得られた酸化チタンの比表面積は150m2g-1であり、実施例2と同程度であったが、ドープされた窒素量は約0.04重量%であり実施例2に比較して減少していた。可視光照射下での光触媒能は実施例2に比較して低かった(図2参照)。
実施例1における加熱処理時に流通させる混合ガスの酸素の濃度を30%とし、加熱処理温度を350℃とした。その余は実施例1と同様とした。XRDを測定したところ、アナターゼ酸化チタンに帰属されるピークのみが観察され、アナターゼ結晶型の酸化チタンであることが確認できた。得られた酸化チタンの比表面積は247m2g-1であった。実施例1と同様可視光照射下での光触媒能を評価したところ、図2に示すように、顕著な分解が観察され、高い光触媒能を示した。ドープされた窒素量は約0.05重量%であった。
実施例3における加熱処理時に流通させる混合ガスの酸素の濃度を20%とした。その余は実施例3と同様とした。XRDを測定したところ、実施例3とほとんど同様なアナターゼ酸化チタンに帰属されるピークのみが観察され、両者の結晶性に大きな差異は認められなかった。得られた酸化チタンの比表面積は248m2g-1であり、実施例2と同程度であったが、ドープされた窒素量は約0.07重量%であり実施例3に比較して増大していたが、可視光照射下での光触媒能は実施例3に比較して低かった(図2参照)。
実施例3における加熱処理時に流通させる混合ガスの酸素の濃度をさらに低く0%(窒素のみ)とした。その余は実施例3と同様とした。XRDを測定したところ、実施例3とほとんど同様なアナターゼ酸化チタンに帰属されるピークのみが観察され、両者の結晶性に大きな差異は認められなかった。得られた酸化チタンの比表面積は258m2g-1であり、実施例2と同程度であったが、ドープされた窒素量は約0.11重量%であり実施例3に比較してさらに増大していたが、可視光照射下での光触媒能は実施例3に比較してさらに低かった(図2参照)。
Claims (6)
- チタンアルコキシドと配位子を有する有機物と触媒とを含む混合溶液を容器中に入れ、その容器中に相対湿度を10%から80%に加湿した不活性ガスである気体を流通させることにより、加水分解と重縮合反応に必要な水分を連続的に供給することによって得られた、層状構造を有し層間に有機配位子が配位しているチタニア/有機複合体を、アンモニア水に浸漬することによって、層間の有機配位子を配位子交換反応によって水酸基に置換し、同時にアンモニウムを層状構造のチタニアの層間に導入することによって得られたチタニアとアンモニウムの複合体を、酸素と不活性ガスの混合比を酸素濃度0%〜100%の範囲で最も高い光触媒能を示す混合比に制御した混合ガス流通下で加熱して、アンモニウムの熱分解により窒素をチタニアにドープすると共にアナターゼに結晶化させることを特徴とする光触媒用酸化チタンの製造方法。
- 前記配位子を有する有機物が炭素数3〜24のアルキル基を有する脂肪族カルボン酸または炭素数6〜30のアリール基を有する芳香族カルボン酸であることを特徴とする請求項1に記載の光触媒用酸化チタンの製造方法。
- 該触媒が、炭素数3〜24のアルキル基を有する脂肪族カルボン酸または炭素数6〜30のアリール基を有する芳香族カルボン酸と炭素数3〜24のアルキル基を有する脂肪族アミンまたは炭素数6〜30のアリール基を有する芳香族アミンを混合したものであることを特徴とする請求項1に記載の光触媒用酸化チタンの製造方法。
- 該アンモニア水が0から100℃で浸漬されることを特徴とする請求項1に記載の光触媒用酸化チタンの製造方法。
- チタンアルコキシドと有機物を含む混合溶液を容器中に入れ、その容器中に相対湿度を10%から80%に加湿した不活性ガスである気体を流通させることにより水分を連続的に供給することによってチタンアルコキシドの加水分解と重縮合反応を進行させ、薄片状チタニアに有機配位子が配位し、規則的な層状構造を形成することを特徴とするチタニア/有機複合体の製造方法。
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