JP5212338B2 - Method for evaluating toluene gas removal performance - Google Patents
Method for evaluating toluene gas removal performance Download PDFInfo
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- JP5212338B2 JP5212338B2 JP2009258978A JP2009258978A JP5212338B2 JP 5212338 B2 JP5212338 B2 JP 5212338B2 JP 2009258978 A JP2009258978 A JP 2009258978A JP 2009258978 A JP2009258978 A JP 2009258978A JP 5212338 B2 JP5212338 B2 JP 5212338B2
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title claims description 150
- 238000000034 method Methods 0.000 title claims description 18
- 239000011148 porous material Substances 0.000 claims description 51
- 239000011941 photocatalyst Substances 0.000 claims description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 39
- 238000005259 measurement Methods 0.000 claims description 12
- 238000000921 elemental analysis Methods 0.000 claims 1
- 239000003610 charcoal Substances 0.000 description 33
- 238000000576 coating method Methods 0.000 description 25
- 239000011248 coating agent Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 19
- 239000000126 substance Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 6
- 238000005507 spraying Methods 0.000 description 6
- 230000000903 blocking effect Effects 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
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- 238000011068 loading method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241001330002 Bambuseae Species 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical class CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
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- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- -1 activated carbon Chemical compound 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- 239000001273 butane Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- FQNHWXHRAUXLFU-UHFFFAOYSA-N carbon monoxide;tungsten Chemical group [W].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] FQNHWXHRAUXLFU-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 1
- VNZQQAVATKSIBR-UHFFFAOYSA-L copper;octanoate Chemical compound [Cu+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O VNZQQAVATKSIBR-UHFFFAOYSA-L 0.000 description 1
- VNGORJHUDAPOQZ-UHFFFAOYSA-N copper;propan-2-olate Chemical compound [Cu+2].CC(C)[O-].CC(C)[O-] VNGORJHUDAPOQZ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
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- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- CRHIAMBJMSSNNM-UHFFFAOYSA-N tetraphenylstannane Chemical compound C1=CC=CC=C1[Sn](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 CRHIAMBJMSSNNM-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、表面上に多数の微細孔を有し該表面上に光触媒を分散した状態で担持した多孔材の、トルエンガスの除去性能を評価する方法に関する。 The present invention relates to a method for evaluating toluene gas removal performance of a porous material having a large number of fine pores on a surface and carrying a photocatalyst on the surface .
従来、表面上に多数の微細孔を有し、該表面上に光触媒を備えた多孔材がある。このような光触媒を備えた多孔材としては、例えば、備長炭、竹炭、椰子殻炭、籾殻炭等の多孔材の表面上に、酸化チタン（ＴｉＯ２）を含有する光触媒を、膜状または層状の状態でコーティングして担持させたものがある（例えば、特許文献１参照）。 Conventionally, there are porous materials having a large number of micropores on the surface and a photocatalyst on the surface. As a porous material provided with such a photocatalyst, for example, a photocatalyst containing titanium oxide (TiO 2 ) on the surface of a porous material such as Bincho charcoal, bamboo charcoal, coconut shell charcoal, rice husk charcoal, or the like There are those coated and supported in this state (for example, see Patent Document 1).
そして、上記光触媒を備えた多孔材によれば、悪臭物質、有機物質等の有害物質は、多孔材の微細孔に吸着されるだけではなく、光触媒による酸化還元反応によって二酸化炭素と水に分解されるため、一般の多孔材と比較すれば、有害物質の除去性能は高くなる。 And according to the porous material provided with the photocatalyst, harmful substances such as malodorous substances and organic substances are not only adsorbed in the micropores of the porous material, but also decomposed into carbon dioxide and water by the oxidation-reduction reaction by the photocatalyst. Therefore, compared with a general porous material, the removal performance of harmful substances is enhanced.
さらに、従来、上記光触媒を備えた多孔材の製造方法としては、酸化チタン（ＴｉＯ２）の前駆体を含有するアナターゼ分散液を多孔材の表面上に塗布した後、さらに焼成することで、多孔材の表面に、高密度で密着性に優れた光触媒膜を形成する方法がある（例えば、特許文献２参照）。 Furthermore, conventionally, as a method for producing a porous material provided with the photocatalyst, an anatase dispersion containing a precursor of titanium oxide (TiO 2 ) is applied on the surface of the porous material, and then further baked to obtain a porous material. There is a method of forming a photocatalytic film having high density and excellent adhesion on the surface of a material (see, for example, Patent Document 2).
しかしながら、従来の光触媒を備えた多孔材では、多孔材の表面が、光触媒によって高密度に密着した膜状または層状の状態で一様にコーティングされているため、多孔材の表面上に有る多数の微細孔が、酸化チタン（ＴｉＯ２）等によって塞がれた状態にあった。
このため、酸化チタン（ＴｉＯ２）等の光触媒による有害物質の分解性能は維持されるとしても、他方、微細孔による有害物質の吸着性能は低下してしまうため、有害物質の除去性能及び除去効率が低くなってしまうという問題がある。
However, in the porous material provided with the conventional photocatalyst, the surface of the porous material is uniformly coated in a film-like or layered state in close contact with the photocatalyst at a high density. The micropores were in a state of being blocked by titanium oxide (TiO 2 ) or the like.
For this reason, even if the decomposition performance of harmful substances by photocatalysts such as titanium oxide (TiO 2 ) is maintained, on the other hand, the adsorption performance of harmful substances by micropores is reduced, so the removal performance and removal efficiency of harmful substances There is a problem that becomes low.
また、従来の光触媒を備えた多孔材の製造方法では、光触媒である酸化チタン（ＴｉＯ２）等を多孔材の表面に担持させるためには、３９０〜５００℃の高温にする必要があるとされているが、実際には、５００℃以上の高温にする必要があった。
このため、焼成に使用し得る炉としては、高温に耐え得るものに限られ、焼成に要するコストが高くなってしまうという問題がある。
Further, in the conventional method for producing a porous material provided with a photocatalyst, it is necessary to increase the temperature to 390 to 500 ° C. in order to carry titanium oxide (TiO 2 ) or the like, which is a photocatalyst, on the surface of the porous material. However, in practice, it was necessary to raise the temperature to 500 ° C. or higher.
For this reason, furnaces that can be used for firing are limited to those that can withstand high temperatures, and there is a problem that the cost required for firing increases.
さらに、光触媒を備えた多孔材のトルエンガスの除去性能を効果的に評価する方法の実現が求められている。Furthermore, realization of a method for effectively evaluating the performance of removing toluene gas from a porous material provided with a photocatalyst is required.
そこで、本発明は、光触媒を備えた多孔材のトルエンガスの除去性能を効果的に評価する方法を提供することを目的とする。 Then, an object of this invention is to provide the method of evaluating effectively the removal performance of the toluene gas of the porous material provided with the photocatalyst.
上記課題を解決するために、本発明は、表面上に多数の微細孔を有し該表面上に光触媒を分散した状態で担持した多孔材の、トルエンガスの除去性能を評価する方法であって、表面上に光触媒を分散した状態で担持した前記多孔材を、トルエンガスを充満させたガスパック中に入れて、所定時間経過後に、トルエンガスの残存濃度を測定する測定工程を、複数回繰り返し、各測定工程における測定結果に基づいて、前記多孔材の、トルエンガスの除去性能を評価する方法であり、前記光触媒を担持した前記多孔材であって当該光触媒の担持量が異なる複数の前記多孔材を準備し、前記複数の多孔材のそれぞれについて、前記測定工程を複数回繰り返し、各測定工程における測定結果に基づいて、それぞれの多孔材の、トルエンガスの除去性能を評価することを特徴とする。
また、前記光触媒としての酸化チタン（ＴｉＯ２）が前記多孔材の表面上に存在する割合を、前記多孔材の表面をエネルギー分散型Ｘ線分析装置（ＥＤＸ）を用いて元素組成分析することによって測定する工程を有することとしてもよい。
In order to solve the above problems, the present invention is a method for evaluating the toluene gas removal performance of a porous material having a large number of fine pores on the surface and carrying a photocatalyst dispersed on the surface. The porous material supported with the photocatalyst dispersed on the surface is placed in a gas pack filled with toluene gas, and the measurement step of measuring the residual concentration of toluene gas after a predetermined time has been repeated a plurality of times. The method for evaluating the removal performance of toluene gas of the porous material based on the measurement results in each measurement step, wherein the porous material supports the photocatalyst, and the plurality of the porous materials differing in the amount of the photocatalyst supported The material is prepared, and for each of the plurality of porous materials, the measurement process is repeated a plurality of times. Evaluation, characterized in that.
Further, by analyzing the element composition of the surface of the porous material using an energy dispersive X-ray analyzer (EDX), the proportion of titanium oxide (TiO 2 ) as the photocatalyst present on the surface of the porous material. It is good also as having the process of measuring.
本発明によれば、表面上に多数の微細孔を有し該表面上に光触媒を分散した状態で担持した多孔材の、トルエンガスの除去性能を効果的に評価する方法を、提供することが可能となる。According to the present invention, it is possible to provide a method for effectively evaluating the toluene gas removal performance of a porous material having a large number of micropores on the surface and carrying a photocatalyst dispersed on the surface. It becomes possible.
以下、添付図面を参照しながら、本発明の光触媒を備えた多孔材を実施するための最良の形態について詳細に説明する。 Hereinafter, the best mode for carrying out a porous material provided with the photocatalyst of the present invention will be described in detail with reference to the accompanying drawings.
なお、本明細書及び図面には、次のような発明も含まれている。
表面上に多数の微細孔を有し、該表面上に光触媒を備えた多孔材であって、光触媒は、微細孔を塞ぐことなく、表面上に分散した状態で担持されていることを特徴とする。特に、光触媒は、微細孔を塞ぐことなく、表面上に点在した状態で担持されていることが好ましい。
ここで、上記多孔材とは、表面に多数の微細孔を有する基材をいい、例えば、活性炭等の多孔質炭素や、多孔質アルミ等の多孔質金属等があり、その他、セルロース、リグニン、キチン、キトサン、天然ゴム、ポリエステル、ポリ塩化ビニル、ポリオレフィン、ポリウレタン、エポキシ樹脂、フェノール樹脂、ゼオライト、シリカゲル、セピオライト、ミズカナイト、アルミナ、ルテニウム、酸化インジウム等がある。また、これらのうち少なくとも１種以上を組み合わせてもよい。
このような多孔材としては、多量の光触媒を多孔材の表面に分散した状態で担持させるという観点からすれば、特に、比表面積が高い、珪藻土、漆喰、籾殻炭、椰子殻炭、竹炭及び備長炭等の木炭うち少なくとも１種以上からなることを特徴とすることが好ましい。
また、上記光触媒とは、光を吸収し、その光エネルギーを他の反応物に与えて各種化学反応（光触媒反応）を誘起し得る物質をいい、例えば、酸化亜鉛（ＺｎＯ）、酸化銅（Ｃｕ ２ Ｏ）、酸化ニッケル（ＮｉＯ）、酸化鉄（Ｆｅ ２ Ｏ ３ ）、チタン酸ストロンチウム（ＳｒＴｉＯ ３ ）、酸化ケイ素（ＳｉＯ ２ ）、酸化タングステン（ＷＯ ３ ）、酸化スズ（ＳｎＯ ２ ）等の金属酸化物や、硫化カドミウム（ＣｄＳ）、硫化亜鉛（ＺｎＳ）等の金属硫化物等がある。また、これらのうち少なくとも１種以上を組み合わせてもよい。
このような光触媒としては、分解性能が高い光触媒を多孔材に担持させるという観点からすれば、特に、光触媒としての活性が高く、多孔材との密着性が高い、酸化チタン（ＴｉＯ ２ ）を含有することを特徴とすることが好ましい。ここで、酸化チタン（ＴｉＯ ２ ）は、アナターゼ型、ブルッカイト型、ルチル型等のうちいずれのタイプであってもよく、また、これらの混晶タイプのものであってもよい。
さらに、上記光触媒は、酸化チタン（ＴｉＯ ２ ）以外にも、光触媒反応を促進させるため、白金（Ｐｔ）、金（Ａｕ）、鉛（Ｐｄ）、ニッケル（Ｎｉ）、鉄（Ｆｅ）等の助触媒を含有してもよい。
また、上記酸化チタン（ＴｉＯ ２ ）は、多孔材の表面を、エネルギー分散型Ｘ線分析装置（ＥＤＸ）を用いて元素組成分析した結果、１０〜４０重量％であることを特徴としてもよく、好ましくは、１０〜３２重量％であり、さらに好ましくは、およそ１２重量％である。
さらに、光触媒を備えた多孔材の製造方法であって、光触媒の前駆体を含有する溶液を多孔材の表面上に接触させた後、一定温度で熱処理する工程を有することを特徴とする。
ここで、上記光触媒の前駆体とは、乾燥、焼成等を施すことによって、光触媒に変化し、もしくは、光触媒を生成する物質をいい、例えば、チタンイソプロポキシド、チタンｎ−ブトキシド、テトラ−ｎ−プロピルオルトチタネート、テトラエチルオルトチタネート、トリエトキシ鉄、テトラエトキシシラン、ジエトキシ亜鉛、タングステンヘキサカルボニル、テトラフェニルスズ、ｎ−オクタン酸銅、ジイソプロポキシ銅等がある。また、これらのうち少なくとも１種以上を組み合わせてもよい。
さらに、上記光触媒の前駆体を含有する溶液を作製するための溶媒としては、例えば、メタン、エタン、プロパン、ブタン、エチレン、プロピレン等の炭化水素、メタノール、エタノール、プロパノール、ブタノール等のアルコール、アセトン、メチルエチルケトン等のケトン類、二酸化炭素、水アンモニア、塩素、クロロホルム、フレオン類等がある。
また、上記接触とは、光触媒の前駆体を多孔材の表面上に接触させることをいい、その方法は問わない。例えば、塗布又は噴霧等の方法があり、スプレー、ディッピング、流動スプレー、刷毛塗り等の方法がある。
また、上記一定温度とは、従来の焼成温度よりも低い温度をいい、例えば、２００〜３００℃である。
さらに、上記工程は、アナターゼ型酸化チタンと、ペルオキソチタン（IV）酸水和物と、ペルオキソチタン水和物とを含有する溶液を、多孔材の表面上に塗布または噴霧した後、２００〜３００℃で焼成することを特徴としてもよい。
＝＝＝酸化チタン（ＴｉＯ２）を担持する備長炭の製造＝＝＝
まず、本実施の形態においては、多孔材である備長炭の表面上に、スプレーを用いて所定の回数だけコーティング液を塗布し、これを２００〜３００℃で焼成することで、酸化チタン（ＴｉＯ２）を担持する備長炭を製造した。ここでは、塗布回数を１回、３回、５回、１０回としたもの及びブランクとして未塗布のものを製造した。
The present specification and drawings include the following inventions.
A porous material having a large number of micropores on the surface and having a photocatalyst on the surface, wherein the photocatalyst is supported in a dispersed state on the surface without blocking the micropores. To do. In particular, the photocatalyst is preferably supported in a state of being scattered on the surface without blocking the micropores.
Here, the porous material refers to a substrate having a large number of fine pores on the surface, for example, porous carbon such as activated carbon, porous metal such as porous aluminum, etc., cellulose, lignin, There are chitin, chitosan, natural rubber, polyester, polyvinyl chloride, polyolefin, polyurethane, epoxy resin, phenol resin, zeolite, silica gel, sepiolite, mizukanite, alumina, ruthenium, indium oxide and the like. Moreover, you may combine at least 1 or more types among these.
As such a porous material, from the viewpoint of carrying a large amount of photocatalyst dispersed in the surface of the porous material, diatomaceous earth, plaster, rice husk charcoal, coconut husk charcoal, bamboo charcoal, and bincho are particularly high in specific surface area. It is preferable to be characterized by comprising at least one of charcoal and other charcoal.
The photocatalyst refers to a substance that can absorb light and give the light energy to other reactants to induce various chemical reactions (photocatalytic reactions). For example, zinc oxide (ZnO), copper oxide (Cu 2 O), nickel oxide (NiO), iron oxide (Fe 2 O 3 ), strontium titanate (SrTiO 3 ), silicon oxide (SiO 2 ), tungsten oxide (WO 3 ), tin oxide (SnO 2 ) and other metals There are oxides and metal sulfides such as cadmium sulfide (CdS) and zinc sulfide (ZnS). Moreover, you may combine at least 1 or more types among these.
As such a photocatalyst, from the viewpoint of supporting a photocatalyst having high decomposition performance on a porous material, particularly, it contains titanium oxide (TiO 2 ), which has high activity as a photocatalyst and high adhesion to the porous material. It is preferable that it is characterized. Here, the titanium oxide (TiO 2 ) may be any type of anatase type, brookite type, rutile type, etc., or may be a mixed crystal type of these.
Furthermore, in addition to titanium oxide (TiO 2 ), the photocatalyst promotes the photocatalytic reaction, so that platinum (Pt), gold (Au), lead (Pd), nickel (Ni), iron (Fe), etc. A catalyst may be contained.
The titanium oxide (TiO 2 ) may be characterized in that the surface of the porous material is 10 to 40% by weight as a result of elemental composition analysis using an energy dispersive X-ray analyzer (EDX). Preferably, it is 10 to 32% by weight, and more preferably about 12% by weight.
Furthermore, it is a method for producing a porous material provided with a photocatalyst, which comprises a step of bringing a solution containing a photocatalyst precursor into contact with the surface of the porous material and then heat-treating it at a constant temperature.
Here, the precursor of the photocatalyst refers to a substance that changes to a photocatalyst by performing drying, firing, or the like, or generates a photocatalyst. For example, titanium isopropoxide, titanium n-butoxide, tetra-n -Propyl orthotitanate, tetraethyl orthotitanate, triethoxy iron, tetraethoxysilane, diethoxy zinc, tungsten hexacarbonyl, tetraphenyl tin, copper n-octanoate, diisopropoxy copper and the like. Moreover, you may combine at least 1 or more types among these.
Furthermore, examples of the solvent for preparing the solution containing the photocatalyst precursor include hydrocarbons such as methane, ethane, propane, butane, ethylene, and propylene, alcohols such as methanol, ethanol, propanol, and butanol, and acetone. And ketones such as methyl ethyl ketone, carbon dioxide, water ammonia, chlorine, chloroform, and freons.
Moreover, the said contact means making the precursor of a photocatalyst contact on the surface of a porous material, The method is not ask | required. For example, there are methods such as coating or spraying, and there are methods such as spraying, dipping, fluid spraying, and brushing.
Moreover, the said constant temperature means temperature lower than the conventional baking temperature, for example, is 200-300 degreeC.
Furthermore, the above-described step is performed by applying or spraying a solution containing anatase-type titanium oxide, peroxotitanium (IV) acid hydrate, and peroxotitanium hydrate onto the surface of the porous material, and then 200 to 300 It is good also as baking at ° C.
=== Production of Bincho charcoal carrying titanium oxide (TiO 2 ) ===
First, in the present embodiment, a coating liquid is applied a predetermined number of times on the surface of Bincho charcoal, which is a porous material, using a spray, and this is baked at 200 to 300 ° C., whereby titanium oxide (TiO 2). Bincho charcoal carrying 2 ) was produced. Here, the number of times of coating was set to 1, 3, 5, and 10 and uncoated materials were manufactured as blanks.
なお、上記エコート製コーティング液は、アナターゼ、ペルオキソチタン（IV）酸水和物、ペルオキソチタン水和物を含有するものであり、この溶液は、表１及び表２に示されるペルオキソチタン酸水溶液（Ｐ−cat．）及びペルオキソ改質アナターゼゾル（Ｐ−cat．ＰＬＵＳ）の混合物（Ｐ−cat．ＭＩＸ）である。
＝＝＝酸化チタン（ＴｉＯ２）の担持状態（ＳＥＭ観察結果）＝＝＝
次に、このようにして製造された酸化チタン（ＴｉＯ２）を担持する備長炭について、走査型電子顕微鏡（ＳＥＭ：Scanning Electron Microscope；ＪＳＭ−５６００ＬＶ）を用いて、酸化チタン（ＴｉＯ２）の担持状態を観察した。なお、前処理として、金（Ａｕ）を２００Å蒸着しており、これをＳＥＭの各倍率（３５倍、２５０倍、５００倍、５５０倍、１０００倍）で観察した。この際、二次電子像及び反射電子像の各々につき、酸化チタンの分布状態を写真に記録した。その際の写真の一部を図１Ａ（未塗布：ブランク）、図１Ｂ（塗布１回）、図１Ｃ（塗布３回）、図１Ｄ（塗布５回）に示す。
=== Supporting state of titanium oxide (TiO 2 ) (result of SEM observation) ===
Next, charcoal carrying the thus produced in the titanium oxide (TiO 2), a scanning electron microscope (SEM: Scanning Electron Microscope; JSM -5600LV) using a supported titanium oxide (TiO 2) The condition was observed. As a pretreatment, gold (Au) was vapor-deposited in 200 mm, and this was observed at each magnification of SEM (35 times, 250 times, 500 times, 550 times, and 1000 times). At this time, the distribution state of titanium oxide was recorded in a photograph for each of the secondary electron image and the reflected electron image. A part of the photograph at that time is shown in FIG. 1A (uncoated: blank), FIG. 1B (one coating), FIG. 1C (three coatings), and FIG. 1D (five coatings).
図１Ａ（ブランク）に示される未塗布の場合（ブランク）と比較すれば明らかなように、塗布１回の場合（図１Ｂ参照）及び塗布３回の場合（図１Ｃ参照）には、いずれも、光触媒である酸化チタン（ＴｉＯ２）が備長炭の表面上に担持されており、しかも、備長炭に存在する数ミクロンの微細孔を塞ぐことなく、分散した状態で担持されていることがわかる。 As is clear when compared with the case of no application (blank) shown in FIG. 1A (blank), both in the case of one application (see FIG. 1B) and in the case of three applications (see FIG. 1C) It can be seen that titanium oxide (TiO 2 ), which is a photocatalyst, is supported on the surface of Bincho charcoal, and is supported in a dispersed state without blocking micropores of several microns existing in Bincho charcoal. .
これに対し、図１Ｄに示される塗布５回の場合には、酸化チタン（ＴｉＯ２）は、備長炭の表面上に膜状または層状の状態で担持されており、備長炭に存在する数ミクロンの微細孔の大部分がコーティング膜で埋められ、塞がった状態にあることがわかる。 On the other hand, in the case of five coatings shown in FIG. 1D, titanium oxide (TiO 2 ) is supported in the form of a film or a layer on the surface of Bincho charcoal, and several microns existing in Bincho charcoal. It can be seen that most of the micropores are filled with the coating film and closed.
なお、図１Ｅには、塗布の場合と噴霧の場合とを比較するため、上記コーティング液を１回噴霧した場合の写真も掲載した。この写真からも、酸化チタン（ＴｉＯ２）は、微細孔を塞ぐことなく、備長炭の表面上を分散した状態で担持されていることがわかる。この場合には、酸化チタン（ＴｉＯ２）は、微細孔を塞ぐことなく、点在した状態で担持されていることがわかる。 In addition, in FIG. 1E, in order to compare the case of application | coating with the case of spraying, the photograph at the time of spraying the said coating liquid once was also published. Also from this photograph, it can be seen that titanium oxide (TiO 2 ) is supported in a dispersed state on the surface of Bincho charcoal without blocking the fine holes. In this case, it can be seen that titanium oxide (TiO 2 ) is supported in a scattered state without closing the fine holes.
＝＝＝酸化チタン（ＴｉＯ２）の担持率（ＥＤＸ分析結果）＝＝＝
さらに、本実施の形態においては、備長炭の表面上に担持された酸化チタン（ＴｉＯ２）の存在割合（担持率）を、エネルギー分散型Ｘ線分析装置（ＥＤＸ or ＥＤＳ：Energy Dispersive X-ray Spectrometer；ＪＥＤ−２２００）を用いて分析した。その分析結果を表３に示す。
Further, in the present embodiment, the existing ratio (support rate) of titanium oxide (TiO 2 ) supported on the surface of Bincho charcoal is determined by using an energy dispersive X-ray analyzer (EDX or EDS: Energy Dispersive X-ray). Spectrometer; JED-2200). The analysis results are shown in Table 3.
表３に示されるように、備長炭の表面上に酸化チタン（ＴｉＯ２）が存在する割合は、コーティング液を１回だけ塗布した場合には約１２％であった。また、３回だけ塗布した場合には約３１％であり、５回だけ塗布した場合には約４０％、１０回だけ塗布した場合には約５２％であった。 As shown in Table 3, the proportion of titanium oxide (TiO 2 ) on the surface of Bincho charcoal was about 12% when the coating solution was applied only once. In addition, it was about 31% when applied only 3 times, about 40% when applied only 5 times, and about 52% when applied only 10 times.
このことから、コーティング液の塗布回数が増加するにつれて、備長炭の表面上における酸化チタン（ＴｉＯ２）の担持率も増加することがわかる。 From this, it can be seen that the supporting rate of titanium oxide (TiO 2 ) on the surface of Bincho charcoal increases as the number of coating liquid application increases.
＝＝＝トルエンガスの除去性能及び除去効率＝＝＝
本実施の形態では、このようにして製造された酸化チタン（ＴｉＯ２）を担持する備長炭について、有害物質であるトルエンガスの除去性能及び除去効率を調べた。ここでは、塗布回数が、１回、３回、５回及びブランクとして未塗布のものを試験体とした。
=== Toluene gas removal performance and removal efficiency ===
In this embodiment, the charcoal carrying the so-produced titanium oxide (TiO 2), was investigated removal performance and removal efficiency of toluene gas is harmful substances. Here, the number of times of application was 1, 3, 5, and a blank that was not applied was used as a test specimen.
その後、各試験体を入れた５Ｌの各ガスバック中にトルエンガスを充満させ、ＵＶランプを点灯後、経時的にトルエンガスの残存濃度を検知管で測定した。なお、試験開始前に、６５〜７０ｐｐｍ程度のトルエンガスで充満させたガスバック中に、各試験体を入れて１８時間静置し、これを飽和状態にしておいた。 Thereafter, each gas bag of 5 L containing each test specimen was filled with toluene gas, the UV lamp was turned on, and the residual concentration of toluene gas was measured with a detector tube over time. In addition, before the test start, each test body was put in the gas bag filled with about 65-70 ppm toluene gas, and left still for 18 hours, and this was made into the saturated state.
このような試験をトルエンガスの初期濃度を変えて３回繰り返した。１回目のトルエンガスの初期濃度は１６０ｐｐｍであり、２回目のトルエンガスの初期濃度は１３０〜１４０ｐｐｍ、３回目のトルエンガスの初期濃度は８０〜１００ｐｐｍであった。その測定結果を試験回数ごとに図２に示す。 Such a test was repeated three times while changing the initial concentration of toluene gas. The initial concentration of the first toluene gas was 160 ppm, the initial concentration of the second toluene gas was 130 to 140 ppm, and the initial concentration of the third toluene gas was 80 to 100 ppm. The measurement results are shown in FIG. 2 for each number of tests.
図２のグラフに示されるように、いずれの各試験回数（１回目，２回目，３回目）においても、塗布回数が少ないものほど、同じ経過時点におけるトルエンガスの残存濃度は低下しており、トルエンガスの除去性能が高いことがわかる。 As shown in the graph of FIG. 2, in any test number (first time, second time, third time), the smaller the number of times of application, the lower the residual concentration of toluene gas at the same time point. It can be seen that the removal performance of toluene gas is high.
すなわち、試験回数が１回目の場合には、塗布回数が１回及び３回のものは、トルエンガスの除去性能は高く、また、塗布回数が５回のものについても、トルエンガスの除去性能は比較的高いことがわかる。なお、ブランクの備長炭は、前処理によって既に飽和状態とされ、吸着性能は限界に達しているため、トルエンガスの除去性能はほとんど認められなかった（図２（ａ）参照）。 That is, when the number of tests is the first time, the performance of removing toluene gas is high when the number of times of coating is 1 and 3, and the performance of removing toluene gas is also when the number of times of coating is 5. It can be seen that it is relatively high. Note that the blank Bincho charcoal was already saturated by the pretreatment, and the adsorption performance reached the limit, so that the toluene gas removal performance was hardly recognized (see FIG. 2A).
さらに、試験回数が２回目の場合には、塗布回数が１回及び３回のものはトルエンガスの除去性能が高いが、他方、塗布回数が５回のものはトルエンガスの除去性能が低下していることがわかる（図２（ｂ）参照）。 Furthermore, when the number of tests is the second time, the performance of removing toluene gas is high when the number of times of coating is 1 and 3 while the performance of removing toluene gas is high when the number of times of coating is 5 times. (See FIG. 2B).
また、試験回数が３回目の場合には、塗布回数が１回及び３回のものはトルエンガスの除去性能が高いが、他方、塗布回数が５回のものはトルエンガスの除去性能が著しく低下していることがわかる（図２（ｃ）参照）。 In addition, when the number of tests is the third time, the performance of removing toluene gas is high when the number of times of coating is 1 and 3, while the performance of removing toluene gas is significantly decreased when the number of times of coating is 5 times. (See FIG. 2C).
さらに、上記測定結果に基づき、各試験開始後、約４００分経過した時点における各塗布回数のトルエンガスの除去効率を算出した。その算出結果を図３に示す。 Furthermore, based on the above measurement results, the removal efficiency of toluene gas was calculated for each number of coatings when about 400 minutes had elapsed after the start of each test. The calculation result is shown in FIG.
ここで、トルエンガスの除去効率は、トルエンガスの初期濃度から測定値を控除することでトルエンガスの除去濃度を求め、これをさらにトルエンガスの初期濃度で除することにより算出した。 Here, the removal efficiency of toluene gas was calculated by obtaining the removal concentration of toluene gas by subtracting the measured value from the initial concentration of toluene gas, and further dividing this by the initial concentration of toluene gas.
図３のグラフに示されるように、コーティング液を塗布したものは、ブランクのものと比べてトルエンガスの除去効率は高くなった。また、塗布回数が少ないものほど、トルエンガスの除去効率は高くなり、さらに、試験回数が少ないものほど、トルエンガスの除去効率は高くなった。 As shown in the graph of FIG. 3, the toluene gas removal efficiency was higher when the coating liquid was applied than when the blank was applied. Moreover, the removal efficiency of toluene gas became higher as the number of application was smaller, and the removal efficiency of toluene gas was higher as the number of tests was smaller.
このことから、コーティング液を備長炭の表面に塗布し、光触媒である酸化チタン（ＴｉＯ２）を担持させることで、微細孔による吸着性能と、光触媒による分解性能とを有するため、トルエンガスの除去効率は高くなることがわかる。但し、塗布回数が増加するにつれて、酸化チタン（ＴｉＯ２）が微細孔を塞いでしまうため、微細孔による吸着性能が低下してしまい、逆に、トルエンガスの除去効率は低くなることがわかる。また、このような備長炭におけるトルエンガスの除去効率は、複数回にわたり継続して維持され得ることもわかる。 From this, the coating liquid is applied to the surface of Bincho charcoal, and by supporting titanium oxide (TiO 2 ), which is a photocatalyst, it has adsorption performance by micropores and decomposition performance by photocatalyst, so removal of toluene gas It turns out that efficiency becomes high. However, it can be seen that as the number of coatings increases, titanium oxide (TiO 2 ) closes the micropores, so that the adsorption performance due to the micropores decreases, and conversely, the toluene gas removal efficiency decreases. Moreover, it turns out that the removal efficiency of toluene gas in such Bincho charcoal can be maintained continuously several times.
以上より、本実施の形態においては、いずれの試験回数においても、塗布回数が１回の場合、すなわち、酸化チタン（ＴｉＯ２）の担持率が約１２重量％の場合に、トルエンガスの除去効率が最も高いことがわかる。また、塗布回数が増加するとともに、トルエンガスの除去効率はしだいに減少し、塗布回数が５回の場合まで、すなわち、酸化チタン（ＴｉＯ２）の担持率が約４０重量％の場合までは、トルエンガスの除去効率は比較的高く維持されていることがわかる。 As described above, in this embodiment, in any number of tests, the removal efficiency of toluene gas when the number of times of coating is 1, that is, when the loading ratio of titanium oxide (TiO 2 ) is about 12% by weight. Is the highest. Further, as the number of times of application increases, the removal efficiency of toluene gas gradually decreases, and until the number of times of application is 5, that is, when the loading ratio of titanium oxide (TiO 2 ) is about 40% by weight, It can be seen that the removal efficiency of toluene gas is maintained relatively high.
したがって、酸化チタン（ＴｉＯ２）の担持率が、エネルギー分散型Ｘ線分析装置（ＥＤＸ）を用いて元素組成分析した結果、約１０〜４０重量％であれば、トルエンガス等の有害物質の分解性能を維持しつつ、微細孔による有害物質の吸着性能を十分に向上させることができ、有害物質の除去性能及び除去効率が高くなると考えられる。その理由としては、酸化チタン（ＴｉＯ２）が、備長炭の微細孔を塞ぐことなく、備長炭の表面上に分散した状態で担持されていることが挙げられる。 Therefore, if the loading ratio of titanium oxide (TiO 2 ) is about 10 to 40% by weight as a result of elemental composition analysis using an energy dispersive X-ray analyzer (EDX), decomposition of harmful substances such as toluene gas While maintaining the performance, the adsorption performance of harmful substances by the fine pores can be sufficiently improved, and it is considered that the removal performance and removal efficiency of the harmful substances are enhanced. The reason for this is that titanium oxide (TiO 2 ) is supported in a dispersed state on the surface of Bincho charcoal without blocking the fine pores of Bincho charcoal.
また、従来の焼成温度（３９０〜５００℃）よりも低温の焼成温度（２００〜３００℃）で、上記性能を有する備長炭を製造することができることもわかる。 Moreover, it turns out that the Bincho charcoal which has the said performance can be manufactured with the calcination temperature (200-300 degreeC) lower temperature than the conventional calcination temperature (390-500 degreeC).
Claims (2)
表面上に光触媒を分散した状態で担持した前記多孔材を、トルエンガスを充満させたガスパック中に入れて、所定時間経過後に、トルエンガスの残存濃度を測定する測定工程を、複数回繰り返し、
各測定工程における測定結果に基づいて、前記多孔材の、トルエンガスの除去性能を評価する方法であり、
前記光触媒を担持した前記多孔材であって当該光触媒の担持量が異なる複数の前記多孔材を準備し、
前記複数の多孔材のそれぞれについて、前記測定工程を複数回繰り返し、
各測定工程における測定結果に基づいて、それぞれの多孔材の、トルエンガスの除去性能を評価することを特徴とする方法。 A method for evaluating the performance of removing toluene gas of a porous material having a large number of micropores on a surface and carrying a photocatalyst dispersed on the surface,
The porous material supported in a state where the photocatalyst is dispersed on the surface is put into a gas pack filled with toluene gas, and after a predetermined time has passed, a measurement step of measuring the residual concentration of toluene gas is repeated a plurality of times,
Based on the measurement results in each measurement step , is a method for evaluating the removal performance of toluene gas of the porous material ,
Preparing a plurality of the porous materials carrying the photocatalyst and having different amounts of the photocatalyst supported;
For each of the plurality of porous materials, the measurement step is repeated a plurality of times,
A method for evaluating the removal performance of toluene gas of each porous material based on measurement results in each measurement step .
前記光触媒としての酸化チタン（ＴｉＯ２）が前記多孔材の表面上に存在する割合を、前記多孔材の表面をエネルギー分散型Ｘ線分析装置（ＥＤＸ）を用いて元素組成分析することによって測定する工程を有することを特徴とする方法。 A method for evaluating the removal performance of toluene gas according to claim 1 ,
The proportion of titanium oxide (TiO 2 ) as the photocatalyst present on the surface of the porous material is measured by elemental analysis of the surface of the porous material using an energy dispersive X-ray analyzer (EDX). A method comprising the steps.
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