JP7392516B2 - photocatalyst - Google Patents
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- JP7392516B2 JP7392516B2 JP2020032998A JP2020032998A JP7392516B2 JP 7392516 B2 JP7392516 B2 JP 7392516B2 JP 2020032998 A JP2020032998 A JP 2020032998A JP 2020032998 A JP2020032998 A JP 2020032998A JP 7392516 B2 JP7392516 B2 JP 7392516B2
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- 239000011941 photocatalyst Substances 0.000 title claims description 33
- 239000013078 crystal Substances 0.000 claims description 16
- 229910010252 TiO3 Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 description 24
- 229910052739 hydrogen Inorganic materials 0.000 description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 23
- 239000007789 gas Substances 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910017682 MgTi Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910002971 CaTiO3 Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- VSQYNPJPULBZKU-UHFFFAOYSA-N mercury xenon Chemical compound [Xe].[Hg] VSQYNPJPULBZKU-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Description
本発明は、光触媒に関する。 The present invention relates to a photocatalyst.
近年、光エネルギーを用いて水を分解し、水素を得るために用いられる光触媒の研究が進められている。光触媒は、より多くの水素を得るために、水の分解活性が高いことが好ましい。 In recent years, research has been progressing on photocatalysts that are used to decompose water using light energy and obtain hydrogen. The photocatalyst preferably has high water decomposition activity in order to obtain more hydrogen.
特許文献１には、ＣａＴｉＯ3で表されるペロブスカイト型酸化物のＣａの一部をＳｒで置換し、Ｃａ1-xＳｒxＴｉＯ3とした光触媒が記載されている。 Patent Document 1 describes a photocatalyst in which a part of Ca in a perovskite-type oxide represented by CaTiO 3 is replaced with Sr to form Ca 1-x Sr x TiO 3 .
しかしながら、特許文献１に記載の光触媒は、ＣａとＳｒが相互に固溶した状態となり、十分な触媒活性が得られない。 However, in the photocatalyst described in Patent Document 1, Ca and Sr are in a solid solution with each other, and sufficient catalytic activity cannot be obtained.
本発明は、上記課題を解決するものであり、活性が高い光触媒を提供することを目的とする。 The present invention solves the above problems, and aims to provide a highly active photocatalyst.
本発明の光触媒は、（ＣａＭｇ）ＴｉＯ3を含む酸化物を備え、
前記（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）は、０より大きく、０．７以下であることを特徴とする。
The photocatalyst of the present invention includes an oxide containing (CaMg) TiO3 ,
The ratio Mg/(Ca+Mg) of the molar amount of Mg to the total molar amount of Ca and Mg contained in the (CaMg)TiO 3 is greater than 0 and less than or equal to 0.7.
本発明の光触媒は活性が高い。したがって、本発明の光触媒を用いて水の分解を行ったときに、より多くの水素を発生させることができる。 The photocatalyst of the present invention has high activity. Therefore, when water is decomposed using the photocatalyst of the present invention, more hydrogen can be generated.
以下に本発明の実施形態を示して、本発明の特徴を具体的に説明する。 Embodiments of the present invention will be shown below, and features of the present invention will be specifically explained.
本発明の光触媒は、（ＣａＭｇ）ＴｉＯ3を含む酸化物を備え、（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）は、０より大きく、０．７以下である。酸化物には、ＣａＴｉＯ3の結晶相とＭｇＴｉＯ3の結晶相が混在しており、ＣａＴｉＯ3とＭｇＴｉＯ3の固溶体は存在しない。 The photocatalyst of the present invention includes an oxide containing (CaMg)TiO 3 , and the ratio of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 is greater than 0. , 0.7 or less. In the oxide, a crystal phase of CaTiO 3 and a crystal phase of MgTiO 3 are mixed, and a solid solution of CaTiO 3 and MgTiO 3 does not exist.
図１は、本発明の一実施形態における光触媒の結晶構造を模式的に示す図である。図１において、「Ａ」で表される結晶相は、ＣａＴｉＯ3の結晶相であり、「Ｂ」で表される結晶相は、ＭｇＴｉＯ3の結晶相であり、「Ｃ」で表される結晶相は、ＭｇＴｉ2Ｏ3の結晶相である。図１に示すように、一実施形態における光触媒には、ＣａＴｉＯ3の結晶相とＭｇＴｉＯ3の結晶相が混在しており、さらに少量のＭｇＴｉ2Ｏ3の結晶相が存在する。ただし、ＭｇＴｉ2Ｏ3の結晶相は存在しない場合もある。 FIG. 1 is a diagram schematically showing the crystal structure of a photocatalyst in an embodiment of the present invention. In FIG. 1, the crystal phase represented by "A" is the crystal phase of CaTiO3 , the crystal phase represented by "B" is the crystal phase of MgTiO3 , and the crystal phase represented by "C" is the crystal phase of CaTiO3. The phase is a crystalline phase of MgTi 2 O 3 . As shown in FIG. 1, in the photocatalyst in one embodiment, a crystal phase of CaTiO 3 and a crystal phase of MgTiO 3 coexist, and a small amount of a crystal phase of MgTi 2 O 3 is also present. However, the MgTi 2 O 3 crystal phase may not exist.
（実施例）
ＴｉＯ2、ＣａＣＯ3、および、ＭｇＣＯ3の原料粉を所望の組成比で調合し、ボールミルで５時間撹拌乾燥し、１１００℃で仮焼してセラミック粉体を得た。得られたセラミック粉体を硝酸Ｎｉ水溶液に浸漬し、撹拌しながら１５０℃のホットプレートで蒸発乾燥させた。その後、大気中５００℃で熱処理することによって硝酸を揮発させた後、水素中８００℃で還元して、Ｎｉを１重量％担持させた（ＣａＭｇ）ＴｉＯ3粉からなる光触媒を作製した。Ｎｉは、助触媒として機能する。ただし、助触媒がＮｉに限定されることはなく、ＰｔやＰｄなどを用いることもできる。
(Example)
Raw material powders of TiO 2 , CaCO 3 , and MgCO 3 were prepared in a desired composition ratio, stirred and dried in a ball mill for 5 hours, and calcined at 1100° C. to obtain ceramic powder. The obtained ceramic powder was immersed in a Ni nitrate aqueous solution and evaporated to dryness on a hot plate at 150° C. while stirring. Thereafter, nitric acid was volatilized by heat treatment at 500° C. in the air, and then reduced at 800° C. in hydrogen to produce a photocatalyst made of (CaMg)TiO 3 powder carrying 1% by weight of Ni. Ni functions as a promoter. However, the co-catalyst is not limited to Ni, and Pt, Pd, etc. can also be used.
作製した光触媒の活性を、以下の方法により評価した。 The activity of the produced photocatalyst was evaluated by the following method.
図２は、光触媒の活性を評価するために用いた装置の構成を模式的に示す図である。シャーレ２１に、作製した光触媒の粉体０．３ｇと純水１ｇを混合して得られるスラリーを入れた。そして、そのシャーレ２１を密封容器２２内に入れた後、石英ガラスからなる蓋２３をして密封した。なお、石英ガラスからなる蓋２３は、紫外線を透過させる。
FIG. 2 is a diagram schematically showing the configuration of an apparatus used to evaluate the activity of a photocatalyst. A slurry obtained by mixing 0.3 g of the prepared photocatalyst powder and 1 g of pure water was placed in a
続いて、１リットルのアルゴンガスを満たしたパック２４から、送風ポンプ２５を用いて、アルゴンガスを送出させて、１ｃｃ／分の量のアルゴンガスを循環させた。すなわち、パック２４内のアルゴンガスを、密封容器２２内を通過して、再びパック２４内へと戻るように循環させた。なお、アルゴンガスは、水の分解により発生した水素が酸素等と反応することを抑制するために、密封容器２２内に導入させた。
Subsequently, the
続いて、石英ガラスからなる蓋２３を介して、シャーレ２１内のスラリーに紫外線を照射した。スラリーに紫外線を照射することによって水の分解が生じ、水素が発生する。この状態を１時間継続し、１時間後の混合ガス中の水素の含有割合をガスクロマトグラフィーにより求めた。混合ガス中の水素の含有割合は、アルゴンと水素の混合ガス中の水素の含有割合を意味する。
Subsequently, the slurry in the
なお、紫外線の照射源として、２００Ｗの水銀キセノンランプを用いた。この水銀キセノンランプは、４ｃｍ□の範囲に均一に紫外線を照射することができるので、平面視で直径が３ｃｍの円形のシャーレ２１の全体に紫外線を照射することが可能である。
Note that a 200 W mercury xenon lamp was used as the ultraviolet irradiation source. This mercury-xenon lamp can uniformly irradiate ultraviolet rays over an area of 4 cm square, so it is possible to irradiate the entire
ここでは、光触媒の（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）を変更したときの水素の発生量を調べた。（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）と、混合ガス中の水素の含有割合との関係を表１に示す。また、（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）を横軸に、混合ガス中の水素の含有割合を縦軸にとったグラフを図３に示す。 Here, the amount of hydrogen generated when changing the ratio Mg/(Ca+Mg) of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 of the photocatalyst was investigated. Table 1 shows the relationship between the ratio Mg/(Ca+Mg) of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 and the content rate of hydrogen in the mixed gas. In addition, a graph is shown in which the horizontal axis is the ratio of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 (Mg/(Ca+Mg)), and the vertical axis is the content ratio of hydrogen in the mixed gas. Shown in Figure 3.
図３に示すように、ＣａとＭｇの合計モル量に対するＭｇのモル量が０より大きく、かつ、０．７以下の範囲では、混合ガス中の水素の割合が０．００５％より多くなった。一方、ＣａＴｉＯ3で表されるペロブスカイト型酸化物のＣａの一部をＳｒで置換し、Ｃａ1-xＳｒxＴｉＯ3とした特許文献１に記載の光触媒を用いた場合、混合ガス中の水素の割合は０．００５％未満となる。 As shown in Figure 3, when the molar amount of Mg relative to the total molar amount of Ca and Mg is greater than 0 and 0.7 or less, the proportion of hydrogen in the mixed gas is greater than 0.005%. . On the other hand, when using the photocatalyst described in Patent Document 1 in which a part of Ca in a perovskite oxide represented by CaTiO 3 is replaced with Sr to make Ca 1-x Sr x TiO 3 , hydrogen in the mixed gas The ratio is less than 0.005%.
すなわち、（ＣａＭｇ）ＴｉＯ3を含む酸化物を備え、（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０より大きく、０．７以下である本発明の光触媒は、触媒活性が高く、水の分解により発生する水素の量が多い。 That is, an oxide containing (CaMg)TiO 3 is provided, and the ratio Mg/(Ca+Mg) of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 is greater than 0 and 0.7 or less. The photocatalyst of the present invention has high catalytic activity and generates a large amount of hydrogen by decomposing water.
ここで、光触媒を用いた水の分解反応について簡単に説明する。光触媒にバンドギャップ以上のエネルギーの光が照射されると、価電子帯の電子が伝導帯へと励起される。励起された電子は、水を還元して水素を生成し、価電子帯に形成されたホールは、水を酸化して酸素を生成する。ただし、形成された電子とホールが引き合って再結合すると、水の分解は行われない。 Here, the water decomposition reaction using a photocatalyst will be briefly explained. When a photocatalyst is irradiated with light with an energy higher than the band gap, electrons in the valence band are excited to the conduction band. The excited electrons reduce water to generate hydrogen, and the holes formed in the valence band oxidize water to generate oxygen. However, if the formed electrons and holes attract each other and recombine, water will not be split.
ここで、ＭｇＴｉＯ3とＣａＴｉＯ3は、バンド構造が若干異なるため、界面でバンドが歪んでいると推定される。このバンドの歪みにより、形成された電子とホールが再結合されにくく、水の分解により水素が生成されやすくなると考えられる。 Here, since MgTiO 3 and CaTiO 3 have slightly different band structures, it is presumed that the band is distorted at the interface. It is thought that this band distortion makes it difficult for the formed electrons and holes to recombine, making it easier for hydrogen to be produced by water decomposition.
なお、ＭｇＴｉＯ3単相およびＣａＴｉＯ3単相では触媒活性が低い。すなわち、本発明の光触媒のように、（ＣａＭｇ）ＴｉＯ3を含む酸化物を備え、ＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０より大きく、０．７以下であるという条件が触媒活性を向上させるために重要である。 Note that the catalytic activity is low in MgTiO 3 single phase and CaTiO 3 single phase. That is, the photocatalyst of the present invention includes an oxide containing (CaMg) TiO3 , and the ratio of the molar amount of Mg to the total molar amount of Ca and Mg, Mg/(Ca+Mg), is greater than 0 and less than or equal to 0.7. This condition is important for improving catalytic activity.
また、上記モル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０．３以上０．７以下である場合には、混合ガス中の水素の含有割合が０．００９％以上とさらに高くなった。したがって、本発明における光触媒は、上記モル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０．３以上０．７以下であることが好ましい。 Further, when the molar ratio Mg/(Ca+Mg) was 0.3 or more and 0.7 or less, the hydrogen content in the mixed gas became even higher, 0.009% or more. Therefore, in the photocatalyst in the present invention, the molar ratio Mg/(Ca+Mg) is preferably 0.3 or more and 0.7 or less.
また、図３に示すように、（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比を０から増加していくと、混合ガス中の水素の含有割合が増加するが、Ｍｇのモル量の割合が０．３７の前後において、水素の含有割合の増加量が大きく変化している。すなわち、ＣａとＭｇの合計モル量に対するＭｇのモル量の割合が０．３７以上になると、混合ガス中の水素の含有割合が急激に増加する。したがって、本発明における光触媒は、上記モル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０．３７以上０．７以下であることがより好ましい。 In addition, as shown in Figure 3, as the ratio of the molar amount of Mg to the total molar amount of Ca and Mg contained in (CaMg)TiO 3 is increased from 0, the content ratio of hydrogen in the mixed gas increases. However, when the molar ratio of Mg is around 0.37, the amount of increase in the hydrogen content ratio changes significantly. That is, when the ratio of the molar amount of Mg to the total molar amount of Ca and Mg becomes 0.37 or more, the content ratio of hydrogen in the mixed gas increases rapidly. Therefore, in the photocatalyst of the present invention, the molar ratio Mg/(Ca+Mg) is more preferably 0.37 or more and 0.7 or less.
また、図３に示すように、ＣａとＭｇの合計モル量に対するＭｇのモル量が０．４３以上０．６３以下の場合には、混合ガス中の水素の含有割合が０．０１６％以上とさらに高くなった。したがって、本発明における光触媒は、上記モル量の比Ｍｇ／（Ｃａ＋Ｍｇ）が０．４３以上０．６３以下であることがより好ましい。 Further, as shown in FIG. 3, when the molar amount of Mg with respect to the total molar amount of Ca and Mg is 0.43 or more and 0.63 or less, the hydrogen content in the mixed gas is 0.016% or more. It got even higher. Therefore, in the photocatalyst of the present invention, the molar ratio Mg/(Ca+Mg) is more preferably 0.43 or more and 0.63 or less.
本発明は、上記実施形態に限定されるものではなく、本発明の範囲内において、種々の応用、変形を加えることが可能である。 The present invention is not limited to the above embodiments, and various applications and modifications can be made within the scope of the present invention.
２１ シャーレ
２２ 密封容器
２３ 蓋
２４ パック
２５ 送風ポンプ
21
Claims (4)
前記（ＣａＭｇ）ＴｉＯ3に含まれるＣａとＭｇの合計モル量に対するＭｇのモル量の比Ｍｇ／（Ｃａ＋Ｍｇ）は、０より大きく、０．７以下であり、
前記酸化物には、ＣａＴｉＯ 3 の結晶相とＭｇＴｉＯ 3 の結晶相が混在していることを特徴とする光触媒。 Comprising an oxide containing (CaMg) TiO3 ,
The ratio Mg/(Ca+Mg) of the molar amount of Mg to the total molar amount of Ca and Mg contained in the (CaMg)TiO 3 is greater than 0 and 0.7 or less,
A photocatalyst characterized in that the oxide contains a mixture of a CaTiO 3 crystal phase and an MgTiO 3 crystal phase.
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| JP2011006292A (en) | 2009-06-26 | 2011-01-13 | Sakai Chem Ind Co Ltd | Titanium dioxide particles and method for producing the same |
| WO2011016527A1 (en) | 2009-08-07 | 2011-02-10 | 株式会社モチガセ | Hydroxyl radical generator, antiviral material using hydroxyl radical generator, and method for generating hydroxyl radicals |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2011006292A (en) | 2009-06-26 | 2011-01-13 | Sakai Chem Ind Co Ltd | Titanium dioxide particles and method for producing the same |
| WO2011016527A1 (en) | 2009-08-07 | 2011-02-10 | 株式会社モチガセ | Hydroxyl radical generator, antiviral material using hydroxyl radical generator, and method for generating hydroxyl radicals |
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