JP2010022958A - Photolysis method - Google Patents
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- JP2010022958A JP2010022958A JP2008188446A JP2008188446A JP2010022958A JP 2010022958 A JP2010022958 A JP 2010022958A JP 2008188446 A JP2008188446 A JP 2008188446A JP 2008188446 A JP2008188446 A JP 2008188446A JP 2010022958 A JP2010022958 A JP 2010022958A
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000006303 photolysis reaction Methods 0.000 title claims abstract description 17
- 230000015843 photosynthesis, light reaction Effects 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007864 aqueous solution Substances 0.000 claims abstract description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007800 oxidant agent Substances 0.000 claims abstract description 20
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 15
- 239000011941 photocatalyst Substances 0.000 claims abstract description 11
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000575 pesticide Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- -1 nitrate ions Chemical class 0.000 description 2
- 0 **(*)c1nc(*)nc(N*)n1 Chemical compound **(*)c1nc(*)nc(N*)n1 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 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
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、光触媒を用いて被分解物を分解する光分解方法に関する。 The present invention relates to a photolysis method for decomposing an object to be decomposed using a photocatalyst.
二酸化チタンを含む光触媒を酸化剤中で使用することにより、被分解物を分解する技術がある。例えば特許文献１には、被処理水に酸化剤として、過酸化水素、オゾン、及び酸素の少なくとも一種を添加することが開示されている。
しかし、酸化剤として過酸化水素、オゾン、又は酸素を用いるのみでは、難分解性の物質は分解できない。本発明は上記事情に鑑みてなされたものであり、その目的とするところは、分解能力が高い光分解方法を提供することにある。 However, by using only hydrogen peroxide, ozone, or oxygen as the oxidizing agent, the hardly decomposable substance cannot be decomposed. The present invention has been made in view of the above circumstances, and an object thereof is to provide a photodecomposition method having a high decomposability.
本発明によれば、酸化剤及び被分解物を含む水溶液中に浸漬された光触媒に光を照射することにより、前記被分解物を光分解する工程を有し、
前記光触媒は、二酸化チタンを含んでおり、
前記水溶液のｐＨは６以上であり、
前記酸化剤として、オゾンを前記水溶液に対して1０重量ｐｐｍ以上５０重量ｐｐｍ以下、酸素を前記水溶液に対して５重量ｐｐｍ以上３０重量ｐｐｍ以下、過酸化水素を前記水溶液に対して２００重量ｐｐｍ以上２５０００重量ｐｐｍ以下含有している光分解方法が提供される。
According to the present invention, there is a step of photolyzing the substance to be decomposed by irradiating the photocatalyst immersed in an aqueous solution containing the oxidizing agent and the substance to be decomposed,
The photocatalyst contains titanium dioxide,
The pH of the aqueous solution is 6 or more,
As the oxidizing agent, ozone is 10 to 50 ppm by weight with respect to the aqueous solution, oxygen is 5 to 30 ppm with respect to the aqueous solution, and hydrogen peroxide is 200 to 200 ppm with respect to the aqueous solution. A photolysis method containing 25000 ppm by weight or less is provided.
本発明によれば、分解能力が高い光分解方法を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the photodecomposition method with high decomposition capability can be provided.
以下、本発明の実施の形態について説明する。本実施形態にかかる光分解方法は、酸化剤及び被分解物を含む水溶液中に浸漬された光触媒に光を照射することにより、被分解物を光分解する工程を有する。本発明者らが鋭意検討を行った結果、光触媒として二酸化チタンを用いた場合、酸化剤として過酸化水素、オゾン、及び酸素の３種類を同時に使用し、これらの濃度を適切な範囲に制御し、かつ水溶液のｐＨを適切な範囲に制御することにより、光分解法の分解能力が高まることを見出した。 Embodiments of the present invention will be described below. The photodecomposition method according to the present embodiment includes a step of photodegrading a substance to be decomposed by irradiating light to a photocatalyst immersed in an aqueous solution containing an oxidizing agent and the object to be decomposed. As a result of intensive studies by the present inventors, when titanium dioxide is used as a photocatalyst, three types of hydrogen peroxide, ozone, and oxygen are simultaneously used as an oxidizing agent, and these concentrations are controlled within an appropriate range. And, it was found that the decomposition ability of the photolysis method is enhanced by controlling the pH of the aqueous solution to an appropriate range.
オゾンの濃度は水溶液に対して１０重量ｐｐｍ以上５０重量ｐｐｍ以下であり、好ましくは２５重量ｐｐｍ以上４０重量ｐｐｍ以下である。酸素の濃度は水溶液に対して５重量ｐｐｍ以上３０重量ｐｐｍ以下であり、好ましくは７重量ｐｐｍ以上３０重量ｐｐｍ以下である。過酸化水素の濃度は水溶液に対して２００重量ｐｐｍ以上２５０００重量ｐｐｍ以下であり、好ましくは３００重量ｐｐｍ以上５０００重量ｐｐｍ以下である。 The concentration of ozone is 10 ppm to 50 ppm by weight with respect to the aqueous solution, preferably 25 ppm to 40 ppm. The concentration of oxygen is 5 to 30 ppm by weight, preferably 7 to 30 ppm by weight with respect to the aqueous solution. The concentration of hydrogen peroxide is 200 to 25000 ppm by weight, preferably 300 to 5000 ppm by weight with respect to the aqueous solution.
水溶液のｐＨは、６以上であり、好ましくは６以上１３以下である。ｐＨが１３超になると、反応装置の腐食が問題になるため、好ましくない。 The pH of the aqueous solution is 6 or more, preferably 6 or more and 13 or less. If the pH exceeds 13, corrosion of the reactor becomes a problem, which is not preferable.
また、水溶液に含まれる二酸化チタンの量は、０.５ｇ／リットル以上８ｇ／リットル以下であるのが好ましい。なお二酸化チタンは、修飾改質されていてもよい。光源としては、例えば水銀灯、キセノンランプ、重水素ランプ、蛍光灯、ブラックライト、及び太陽光の少なくとも一つを用いることができる。 The amount of titanium dioxide contained in the aqueous solution is preferably 0.5 g / liter or more and 8 g / liter or less. Titanium dioxide may be modified and modified. As the light source, for example, at least one of a mercury lamp, a xenon lamp, a deuterium lamp, a fluorescent lamp, a black light, and sunlight can be used.
本実施形態によれば、光分解法の分解能力を高めることができる。このため、例えば被分解物がトリアジン系農薬であったとしても、トリアジン系農薬をシアヌル酸、水、二酸化炭素、硝酸イオン及びアンモニウムイオンに分解し、さらに難分解性の中間生成物であるシアヌル酸を水、二酸化炭素、硝酸イオン及びアンモニウムイオンに分解することができる。その結果、トリアジン系農薬の有機炭素を、すべて無機化合物である二酸化炭素に変えることができる。 According to this embodiment, the decomposition capability of the photolysis method can be enhanced. For this reason, even if the decomposed product is a triazine pesticide, for example, the triazine pesticide is decomposed into cyanuric acid, water, carbon dioxide, nitrate ion and ammonium ion, and cyanuric acid which is a hardly decomposable intermediate product. Can be decomposed into water, carbon dioxide, nitrate ions and ammonium ions. As a result, the organic carbon of the triazine-based pesticide can be changed to carbon dioxide, which is an inorganic compound.
なお、トリアジン系農薬は、下記一般式（１）
（式中、ＸはＣｌ、Ｂｒ、ＯＣＨ３、又はＳＣＨ３を表す。Ｒ１は、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。Ｒ２は、Ｈ、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。Ｒ３は、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。）
で示される構造を１種以上有する化合物を含有している。
Triazine pesticides are represented by the following general formula (1)
(In the formula, X represents Cl, Br, OCH 3 , or SCH 3. R 1 represents CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2. R 2 represents H, CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2 represents R 3 represents CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2 . To express.)
The compound which has 1 or more types of structures shown by is contained.
（実施例１）
水５０ｍＬに、トリアジン系農薬の分解反応の中間生成物であるシアヌル酸０．０５ｍｍｏｌを溶解させた水溶液を準備した。この水溶液及び二酸化チタンを反応器の中にいれ、酸化剤の導入及び光の照射を行いつつ、マグネチックスターラーで攪拌することにより、２４時間ほど光分解を行った。光源としては水銀灯を用いた。なお、酸化剤の組成、二酸化チタンの量、及び水溶液のｐＨを変えることにより、実施例及び比較例の実験を行った。表１に、各実施例及び比較例における実験条件及びシアヌル酸の分解率を示す。
Example 1
An aqueous solution in which 0.05 mmol of cyanuric acid, which is an intermediate product of the decomposition reaction of the triazine-based pesticide, was dissolved in 50 mL of water was prepared. The aqueous solution and titanium dioxide were placed in a reactor, and the mixture was stirred with a magnetic stirrer while introducing an oxidizing agent and irradiated with light, and photolysis was performed for about 24 hours. A mercury lamp was used as the light source. In addition, the experiment of the Example and the comparative example was conducted by changing the composition of the oxidizing agent, the amount of titanium dioxide, and the pH of the aqueous solution. Table 1 shows the experimental conditions and the decomposition rate of cyanuric acid in each example and comparative example.
実施例である試料１〜６において、水溶液のｐＨを１２とした。また、試料１〜５において二酸化チタンの量を２ｇ／Ｌとして、試料６において二酸化チタンの量を０．６ｇ／Ｌとした。 In Samples 1 to 6 as examples, the pH of the aqueous solution was set to 12. In Samples 1 to 5, the amount of titanium dioxide was 2 g / L, and in Sample 6 the amount of titanium dioxide was 0.6 g / L.
そして、試料１では、シアヌル酸の分解率は１００％であった。このときの酸化剤の組成は、オゾン（Ｏ３）が２５重量ｐｐｍ、酸素（Ｏ２）が７重量ｐｐｍ、過酸化水素（Ｈ２Ｏ２）が５４４重量ｐｐｍであった。 In Sample 1, the decomposition rate of cyanuric acid was 100%. The composition of the oxidizing agent at this time was 25 ppm by weight of ozone (O 3 ), 7 ppm by weight of oxygen (O 2 ), and 544 ppm by weight of hydrogen peroxide (H 2 O 2 ).
また、試料２，３ではシアヌル酸の分解率は７０％であった。このときの酸化剤の組成は、過酸化水素が２４０重量ｐｐｍ、２０４００重量ｐｐｍであった点を除いて、試料１と同様であった。 In Samples 2 and 3, the decomposition rate of cyanuric acid was 70%. The composition of the oxidizing agent at this time was the same as that of Sample 1 except that hydrogen peroxide was 240 ppm by weight and 20400 ppm by weight.
また、試料４，５ではシアヌル酸の分解率は８０％であった。このときの酸化剤の組成は、過酸化水素が３１０重量ｐｐｍ、４４２０重量ｐｐｍであった点を除いて、試料１と同様であった。 In Samples 4 and 5, the decomposition rate of cyanuric acid was 80%. The composition of the oxidizing agent at this time was the same as that of Sample 1 except that hydrogen peroxide was 310 ppm by weight and 4420 ppm by weight.
また試料６では、二酸化チタンの量が少ないにもかかわらず、シアヌル酸の分解率は４４％であった。なお酸化剤の組成は、試料１と同様である。 In Sample 6, although the amount of titanium dioxide was small, the decomposition rate of cyanuric acid was 44%. The composition of the oxidizing agent is the same as that of sample 1.
一方、比較例である試料７では、酸化剤にはオゾンが２５重量ｐｐｍ、酸素が７重量ｐｐｍ含まれていたが、過酸化水素が含まれていなかったため、他の条件が試料１と同様であったにもかかわらず、シアヌル酸の分解率は４０％であった。 On the other hand, in the sample 7 as a comparative example, the oxidant contained 25 ppm by weight of ozone and 7 ppm by weight of oxygen, but did not contain hydrogen peroxide. Nevertheless, the degradation rate of cyanuric acid was 40%.
また比較例である試料８では、水溶液のｐＨが４であったため、他の実験条件が試料１と同様であったにもかかわらず、シアヌル酸の分解率は０％であった。 In Sample 8 as a comparative example, since the pH of the aqueous solution was 4, the degradation rate of cyanuric acid was 0% even though the other experimental conditions were the same as Sample 1.
また比較例である試料９では、酸化剤には酸素が７重量ｐｐｍ含まれていたが、オゾン及び過酸化水素が含まれていなかったため、他の条件が試料１と同様であったにもかかわらず、シアヌル酸の分解率は３０％であった。
In Sample 9 which is a comparative example, the oxidant contained 7 ppm by weight of oxygen, but did not contain ozone or hydrogen peroxide, so the other conditions were the same as in Sample 1. The decomposition rate of cyanuric acid was 30%.
（実施例２）
実施例１の試料１と同様の条件において、二酸化チタンの量を変化させることにより、ビスフェノールＡの分解反応速度定数を測定した。結果を図１のグラフに示す。このグラフから、試料１と同様の条件においては、ビスフェノールＡの分解速度定数は、二酸化チタンの濃度が２ｇ／Ｌのときが最も大きいことがわかった。
(Example 2)
Under the same conditions as Sample 1 of Example 1, the decomposition reaction rate constant of bisphenol A was measured by changing the amount of titanium dioxide. The results are shown in the graph of FIG. From this graph, it was found that under the same conditions as Sample 1, the decomposition rate constant of bisphenol A was the highest when the concentration of titanium dioxide was 2 g / L.
Claims (4)
前記光触媒は、二酸化チタンを含んでおり、
前記水溶液のｐＨは６以上であり、
前記酸化剤として、オゾンを前記水溶液に対して1０重量ｐｐｍ以上５０重量ｐｐｍ以下、酸素を前記水溶液に対して５重量ｐｐｍ以上３０重量ｐｐｍ以下、過酸化水素を前記水溶液に対して２００重量ｐｐｍ以上２５０００重量ｐｐｍ以下含有している光分解方法。 Irradiating light to a photocatalyst immersed in an aqueous solution containing an oxidizing agent and a substance to be decomposed, and having a step of photolyzing the substance to be decomposed,
The photocatalyst contains titanium dioxide,
The pH of the aqueous solution is 6 or more,
As the oxidizing agent, ozone is 10 to 50 ppm by weight with respect to the aqueous solution, oxygen is 5 to 30 ppm with respect to the aqueous solution, and hydrogen peroxide is 200 to 200 ppm with respect to the aqueous solution. A photolysis method containing 25000 ppm by weight or less.
前記水溶液のｐＨは１３以下である光分解方法。 The photolysis method according to claim 2,
The photolysis method wherein the pH of the aqueous solution is 13 or less.
前記被分解物は、下記一般式（１）
（式中、ＸはＣｌ、Ｂｒ、ＯＣＨ３、又はＳＣＨ３を表す。Ｒ１は、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。Ｒ２は、Ｈ、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。Ｒ３は、ＣＨ３、Ｃ２Ｈ５、Ｃ３Ｈ７、又はＣＨ（ＣＨ３）２を表す。）
で示される構造を１種以上有する化合物を含有する光分解方法。 In the photolysis method according to any one of claims 1 to 3,
The decomposition target is represented by the following general formula (1)
(In the formula, X represents Cl, Br, OCH 3 , or SCH 3. R 1 represents CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2. R 2 represents H, CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2 represents R 3 represents CH 3 , C 2 H 5 , C 3 H 7 , or CH (CH 3 ) 2 . To express.)
The photolysis method containing the compound which has 1 or more types of structures shown by these.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011152338A1 (en) | 2010-06-04 | 2011-12-08 | 株式会社昭和 | Decomposition/elimination method using a photocatalytic material |
| WO2014178144A1 (en) * | 2013-05-02 | 2014-11-06 | 株式会社フォーティー科研 | Oil treating agent, method for producing same and method for treating oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011152338A1 (en) | 2010-06-04 | 2011-12-08 | 株式会社昭和 | Decomposition/elimination method using a photocatalytic material |
| JP2012011372A (en) * | 2010-06-04 | 2012-01-19 | Showa:Kk | Decomposition/elimination method using photocatalytic material |
| CN102985167A (en) * | 2010-06-04 | 2013-03-20 | 株式会社昭和 | Decomposition/elimination method using a photocatalytic material |
| US8597603B2 (en) | 2010-06-04 | 2013-12-03 | Showa Co., Ltd. | Decomposition/elimination method using a photocatalytic material |
| KR101407444B1 (en) * | 2010-06-04 | 2014-06-13 | 가부시키가이샤 쇼와 | Decomposition/elimination method using a photocatalytic material |
| WO2014178144A1 (en) * | 2013-05-02 | 2014-11-06 | 株式会社フォーティー科研 | Oil treating agent, method for producing same and method for treating oil |
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