JP2008246355A - Photocatalytic reaction apparatus - Google Patents
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- 238000013032 photocatalytic reaction Methods 0.000 title claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 71
- 239000011941 photocatalyst Substances 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 22
- 230000005587 bubbling Effects 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000009529 body temperature measurement Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 40
- 238000012360 testing method Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000004817 gas chromatography Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920002620 polyvinyl fluoride Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006757 chemical reactions by type Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
Abstract
Description
本発明は、光触媒反応装置に関し、詳細にはCO2を光触媒で有機物に固定する試験装置として好適な光触媒反応装置に関する。 The present invention relates to a photocatalytic reaction device, and more particularly to a photocatalytic reaction device suitable as a test device for fixing CO 2 to an organic substance with a photocatalyst.
光触媒は各種分野において幅広く利用されている。近年、CO2の排出量を削減することが地球環境の保護の大きな課題となっているが、CO2化学固定化方法の一つとして、光触媒反応を利用したCO2の還元がある。 Photocatalysts are widely used in various fields. In recent years, reducing CO 2 emissions has become a major issue for the protection of the global environment. One of the CO 2 chemical immobilization methods is reduction of CO 2 using a photocatalytic reaction.
(反応式の例)
(Example of reaction formula)
しかしながら、光触媒を活性化させるためには該光触媒が励起する光の照射が必要である。光触媒を活性化させるために、紫外線発光ダイオード(以下、「UV-LED」と称することがある。)を利用することは良く知られているところであり、光触媒とUV-LEDを組み合わせた例として、浄水タンク及び浄水ポット(特許文献1)、空気清浄装置(特許文献2,3)、内燃機関の排出ガス浄化装置(特許文献4)、冷蔵庫(特許文献5)、生ゴミ処置装置(特許文献6)等が提案されている。
本発明は、CO2を光触媒反応により固定化し、有用な有機物や燃料へ転換するための反応試験に供するのに好適な光触媒反応装置を提供することを課題とする。 An object of the present invention is to provide a photocatalytic reaction apparatus suitable for immobilizing CO 2 by a photocatalytic reaction and using it for a reaction test for conversion to useful organic matter or fuel.
前記課題を解決するため、本発明者らはこれまで、CO2を光触媒反応により固定化する光反応プロセスを評価するための反応試験装置として、加圧反応型、ボックス型(上部照射もしくは側面照射)、ガス循環型などを考案し、試験に供した。しかし、紫外線強度が不充分なため紫外線照射効率が劣る、温度の影響があるため試験条件が限定されるなど不都合があった。そして、CO2化学固定化における触媒反応の評価、引いてはCO2の有機物固定反応における化学固定化反応プロセスを評価する装置として、UV-LED照射装置が好適であることを見出し、更にそれらの配置方法を構築することにより、本発明に到達した。 In order to solve the above-mentioned problems, the present inventors have so far adopted a pressure reaction type, a box type (top irradiation or side irradiation) as a reaction test apparatus for evaluating a photoreaction process in which CO 2 is immobilized by a photocatalytic reaction. ), A gas circulation type was devised and used for testing. However, there are inconveniences such as inferior UV irradiation efficiency due to insufficient UV intensity and limited test conditions due to temperature effects. The evaluation of the catalytic reaction in the CO 2 chemical immobilization, as an apparatus for evaluating a chemical immobilization reaction processes in organic matter fixation reaction of CO 2 is pulled, found that UV-LED illumination device is suitable, further their The present invention has been reached by constructing an arrangement method.
すなわち、本発明は以下の通りである。
(1)光触媒を用いて反応を行う光触媒反応装置において、前記光触媒を励起させる光源として紫外線発光ダイオードを用い、該紫外線発光ダイオードを反応容器の周りに内面方向へ設置すると共に、反応容器内に外面方向へ設置したことを特徴とする光触媒反応装置、
(2)前記反応容器の周りの紫外線発光ダイオードが、多面構造に組まれて配置されている、前記(1)に記載の光触媒反応装置、
(3)前記反応容器内の紫外線発光ダイオードが、反応容器内に設置された上部開口容器の中に多面構造に組まれて設置されており、該上部開口容器の周りに冷却装置が設置されている、前記(1)に記載の光触媒反応装置、
(4)前記反応容器は、温度測定手段と、原料ガス導入口と、ガス排出口とを有し、導入した原料ガスをバブリングする原料ガスバブリング装置を備えている、前記(1)〜(3)のいずれかに記載の光触媒反応装置、
(5)さらに、反応容器内の光触媒を分散する触媒分散手段を備えている、前記(1)〜(4)のいずれかに記載の光触媒反応装置。
(6)さらに、反応容器内の溶媒を撹拌する撹拌手段を備えている、前記(1)〜(5)のいずれかに記載の光触媒反応装置。
(7)さらに、紫外線遮蔽保護カバーを備えている、前記(1)〜(6)のいずれかに記載の光触媒反応装置、及び、
(8)CO2固定化反応に用いる、前記(1)〜(7)のいずれかに記載の光触媒反応装置。
That is, the present invention is as follows.
(1) In a photocatalytic reaction apparatus that performs a reaction using a photocatalyst, an ultraviolet light-emitting diode is used as a light source for exciting the photocatalyst, and the ultraviolet light-emitting diode is installed around the reaction vessel in an inner surface direction, Photocatalytic reactor characterized by being installed in the direction,
(2) The photocatalytic reaction device according to (1), wherein the ultraviolet light-emitting diodes around the reaction vessel are arranged in a multi-face structure,
(3) The ultraviolet light emitting diode in the reaction vessel is installed in a multi-sided structure in an upper opening vessel installed in the reaction vessel, and a cooling device is installed around the upper opening vessel. The photocatalytic reaction device according to (1),
(4) The said reaction container has a raw material gas bubbling apparatus which has a temperature measurement means, a raw material gas inlet, and a gas outlet, and bubbles the introduced raw material gas, (1)-(3 ) The photocatalytic reaction device according to any one of
(5) The photocatalytic reaction device according to any one of (1) to (4), further comprising catalyst dispersion means for dispersing the photocatalyst in the reaction vessel.
(6) The photocatalytic reaction device according to any one of (1) to (5), further comprising stirring means for stirring the solvent in the reaction vessel.
(7) The photocatalytic reaction device according to any one of (1) to (6), further comprising an ultraviolet shielding protective cover, and
(8) The photocatalytic reaction device according to any one of (1) to (7), which is used for a CO 2 fixation reaction.
本発明に係る光触媒反応装置によれば、加圧反応型、ボックス型(紫外線上部照射型もしくは側面照射型)、ガス循環型装置に比べて、消費電力が少ない、紫外線強度が高い、紫外線照射効率が良い、温度の影響を受け難い、光触媒反応装置を提供できる。 According to the photocatalytic reaction device of the present invention, compared with a pressure reaction type, a box type (ultraviolet upper irradiation type or side irradiation type), and a gas circulation type device, the power consumption is low, the ultraviolet intensity is high, and the ultraviolet irradiation efficiency is high. However, it is possible to provide a photocatalytic reaction device that is good and hardly affected by temperature.
また、反応容器の周りの紫外線発光ダイオードが多面構造に組まれて配置されているため、照射効率も良好である。それの裏面を透明樹脂板で覆うことにより、装置取扱時の感電・漏電を防止できる。 Further, since the ultraviolet light emitting diodes around the reaction vessel are arranged in a multi-face structure, the irradiation efficiency is also good. By covering the back surface of the device with a transparent resin plate, it is possible to prevent electric shock and electric leakage when handling the device.
また、反応容器内の紫外線発光ダイオードが、反応容器内に設置した上部開口容器の中に多面構造に組まれて設置され、該上部開口容器の周囲には、該紫外線発光ダイオードを冷却する冷却装置が設置されているため、内部から紫外線を安定照射できると共に、反応温度を一定に保つ効果が有る。 In addition, an ultraviolet light emitting diode in the reaction vessel is installed in a multi-sided structure in an upper opening vessel installed in the reaction vessel, and a cooling device for cooling the ultraviolet light emitting diode around the upper opening vessel Since it is installed, it is possible to stably irradiate ultraviolet rays from the inside and to keep the reaction temperature constant.
また、反応容器内に導入する原料ガスをバブリングする原料ガスバブリング装置を備えているため、原料ガスと光触媒の接触機会が大きい。自在に変形するエアストーンを使用することにより、微細泡にてガスを供給することができる。反応後のガスをガス排出口から排出して組成分析すれば反応率を求めることができるので、光触媒と原料ガスの反応性を迅速に把握可能となる。 Moreover, since the raw material gas bubbling device for bubbling the raw material gas introduced into the reaction vessel is provided, the contact opportunity between the raw material gas and the photocatalyst is large. By using freely deformable air stones, gas can be supplied with fine bubbles. Since the reaction rate can be obtained by discharging the gas after the reaction from the gas outlet and analyzing the composition, the reactivity between the photocatalyst and the raw material gas can be quickly grasped.
さらに、反応容器内の光触媒を分散する分散手段と、反応容器内の溶媒を撹拌する撹拌装置を、各々単独でまたは併用して備えることにより、光触媒の分散が良好になる。光触媒による水の分解試験では良好に水素を発生させることができた。 Furthermore, the dispersion of the photocatalyst in the reaction vessel and the stirrer for stirring the solvent in the reaction vessel are each provided alone or in combination, whereby the photocatalyst is favorably dispersed. In the water decomposition test using a photocatalyst, hydrogen could be generated satisfactorily.
さらに、紫外線遮蔽保護カバーを備えているため、紫外線発光ダイオードより照射される紫外線の人体などへの影響を排除することができる。 Furthermore, since the ultraviolet shielding protective cover is provided, it is possible to eliminate the influence of ultraviolet rays irradiated from the ultraviolet light emitting diodes on the human body.
本発明に係る光触媒反応装置をCO2固定化反応に用いることにより、CO2化学固定化における触媒反応の評価を迅速に行うことが可能になる。 By using the photocatalytic reaction apparatus according to the present invention for the CO 2 fixation reaction, it is possible to quickly evaluate the catalytic reaction in the CO 2 chemical fixation.
以下、本発明の光触媒反応装置の好ましい実施形態を、図面を参照しつつ詳細に説明する。 Hereinafter, preferred embodiments of the photocatalytic reaction device of the present invention will be described in detail with reference to the drawings.
図1は、本発明に係る光触媒反応装置の外観図である。光触媒反応装置には、反応容器外部より紫外線を照射する装置として、反応容器1の周りにUV照射用のUV-LED(日亜化学社製NSHU550B)3のランプが288個、設置されている。このUV-LED3は、基板(80mm×70mm)を6面構造に組み、内面方向へUV-LEDを設置したものである。図1では、UV-LED3を反応容器1の周りに6面構造に組んだ例を示したが、多面構造に組むことで、反応容器内の光触媒に万遍なく紫外線を照射することができる。また、UV-LED3の基板裏面は透明樹脂板(テフロン(登録商標)板、塩化ビニル樹脂板など)2で覆われているため、感電や漏電を防止できる。基板の過熱防止のためには、放熱対策として送風器による空冷処理を行うのがよい。 FIG. 1 is an external view of a photocatalytic reaction device according to the present invention. In the photocatalytic reaction device, 288 UV-LED (NSHU550B manufactured by Nichia Corporation) 3 lamps for UV irradiation are installed around the reaction vessel 1 as a device for irradiating ultraviolet rays from the outside of the reaction vessel. This UV-LED 3 is obtained by assembling a substrate (80 mm × 70 mm) into a six-sided structure and installing the UV-LED in the inner surface direction. Although FIG. 1 shows an example in which the UV-LED 3 is assembled in a six-sided structure around the reaction vessel 1, the photocatalyst in the reaction vessel can be uniformly irradiated with ultraviolet rays by being assembled in a multi-sided structure. Moreover, since the back surface of the substrate of the UV-LED 3 is covered with a transparent resin plate (Teflon (registered trademark) plate, vinyl chloride resin plate, etc.) 2, it is possible to prevent electric shock and electric leakage. In order to prevent overheating of the substrate, it is preferable to perform an air cooling process using a blower as a heat dissipation measure.
また、光触媒反応装置には、反応容器内部より紫外線を照射する装置として、反応容器1の内部にUV照射用のUV-LED(日亜化学社製NSHU550B)5のランプが48個、配置されている。このUV-LEDランプは、上部が開口した円筒容器(内径35mm×高さ100mm)4の中にUV-LED5の基板を設置し、反応容器内部よりUV-LED光を照射できる構造とするため、基板(70mm×20mm)を3面構造に組み、外面方向へUV-LEDを設置したものである。円筒容器の上部は漏電防止のためシリコン栓で密閉されている。図1では、UV-LED5を3面構造に組んだ例を示したが、4面〜6面構造にしてもよい。 Further, in the photocatalytic reaction apparatus, as a device for irradiating ultraviolet rays from the inside of the reaction vessel, 48 UV-LED (Nichia Chemical NSHU550B) 5 lamps for UV irradiation are arranged inside the reaction vessel 1. Yes. This UV-LED lamp has a structure in which the substrate of UV-LED 5 is installed in a cylindrical container (inner diameter 35 mm × height 100 mm) 4 opened at the top, and can be irradiated with UV-LED light from inside the reaction container. A substrate (70 mm × 20 mm) is assembled into a three-surface structure, and UV-LEDs are installed in the outer surface direction. The upper part of the cylindrical container is sealed with a silicon stopper to prevent leakage. Although FIG. 1 shows an example in which the UV-LED 5 is assembled in a three-sided structure, a four-sided to six-sided structure may be used.
反応容器1内の温度制御のためには、上述した円筒容器4の周りに冷却手段6を設置し、冷却水を循環させてUV-LED5の発熱による温度上昇を制御するのが良い。図1では、円筒容器4の周りに冷却水を循環させるためのコイルを巻回した例を示した。 In order to control the temperature in the reaction vessel 1, it is preferable to install a cooling means 6 around the above-described cylindrical vessel 4 and circulate cooling water to control the temperature rise due to heat generation of the UV-LED 5. In FIG. 1, the example which wound the coil for circulating a cooling water around the cylindrical container 4 was shown.
図1では、反応容器1として、円筒形のガラス製4つ口セパラブルフラスコ(内径85mm×高さ115mm、容量500ml)を用いているが、反応容器の形状及び材質はこれに限定されるものではなく、UV透過性の材質であれば樹脂製の反応容器であってもよい。前記の反応容器1は、原料ガス導入口7と、ガス排出口8と、温度測定手段9とを有し、導入した原料ガスをバブリングする原料ガスバブリング装置11を備えている。図1において、10はUV−LED用の電源の配線である。 In FIG. 1, a cylindrical glass four-necked separable flask (inner diameter 85 mm × height 115 mm, capacity 500 ml) is used as the reaction vessel 1, but the shape and material of the reaction vessel are limited to this. Instead, a resin reaction vessel may be used as long as it is a UV transparent material. The reaction vessel 1 has a raw material gas bubbling device 11 that has a raw material gas inlet 7, a gas outlet 8, and a temperature measuring means 9, and that bubbles the introduced raw material gas. In FIG. 1, reference numeral 10 denotes a power supply wiring for the UV-LED.
反応容器1内の温度は、温度測定手段(温度計、熱電対など)9で測定可能である。原料ガスバブリング装置11は、反応容器1内に設置する。設置の仕方は任意であるが、光触媒との接触機会をできるだけ増やすために、図1に示すように、反応容器1の底部からバブリングガスが上昇するように設置することが好ましい。バブリング装置の形状及び気泡の大きさは特に限定されないが、自在に変形するエアストーン等を使用することにより微細泡にてガスを供給することができるので、好ましい。反応容器内で反応したガスと未反応の原料ガスは、ガス排出口8を介して系外に排出する。 The temperature in the reaction vessel 1 can be measured by a temperature measuring means (thermometer, thermocouple, etc.) 9. The raw material gas bubbling device 11 is installed in the reaction vessel 1. Although the installation method is arbitrary, in order to increase the chance of contact with the photocatalyst as much as possible, it is preferable that the bubbling gas rises from the bottom of the reaction vessel 1 as shown in FIG. The shape of the bubbling device and the size of the bubbles are not particularly limited, but it is preferable because gas can be supplied with fine bubbles by using freely deformable air stones or the like. The gas reacted in the reaction vessel and the unreacted raw material gas are discharged out of the system through the gas discharge port 8.
排出された反応ガスは、捕集され、ガスクロマトグラフィー(GC)、フーリエ変換赤外分光計(FT-IR)等で組成分析される。既知の原料ガス組成と、分析で求めた反応ガス組成とから、本発明の光触媒反応装置における応率を求めることができる。そのため、光触媒と原料ガスとの反応性を迅速に把握することができる。 The discharged reaction gas is collected and subjected to composition analysis by gas chromatography (GC), Fourier transform infrared spectrometer (FT-IR) or the like. The response rate in the photocatalytic reaction device of the present invention can be obtained from the known raw material gas composition and the reaction gas composition obtained by analysis. Therefore, it is possible to quickly grasp the reactivity between the photocatalyst and the raw material gas.
本発明の光触媒反応装置においては、光触媒と原料ガスとの接触機会を増やすために、反応容器内の光触媒を分散する分散手段(例えば、超音波発振装置)と、反応容器内の溶媒を撹拌する撹拌手段(スラーラー、撹拌機)を備えていることが好ましい。図1では、簡易で使い易く入手も容易であることから、分散手段と撹拌手段を兼備している市販の超音波スターラー12を用いた例を示した。 In the photocatalytic reaction device of the present invention, in order to increase the chance of contact between the photocatalyst and the raw material gas, a dispersion means (for example, an ultrasonic oscillation device) for dispersing the photocatalyst in the reaction vessel and a solvent in the reaction vessel are agitated. It is preferable to have a stirring means (slurrer, stirrer). FIG. 1 shows an example using a commercially available ultrasonic stirrer 12 having both a dispersing means and a stirring means because it is simple, easy to use and easily available.
上記の光触媒反応装置は、UV-LEDにより発生する紫外線の人体などへの影響を排除するため、UV遮蔽保護カバーを備えていることが好ましい。図1では、(株)クラレ製 コモグラス(UV98%カット)製のUV遮蔽保護カバー13を設けた例を示した。 The photocatalytic reaction device preferably includes a UV shielding protective cover in order to eliminate the influence of ultraviolet rays generated by the UV-LED on the human body. In FIG. 1, the example which provided the UV shielding protective cover 13 made from Kuraray Co., Ltd. comoglass (UV98% cut) was shown.
次に、本発明を実施例により図面を参照しつつ詳細に説明するが、本発明は以下の実施例にのみ限定されるものではない。 EXAMPLES Next, although an Example demonstrates this invention in detail, referring drawings, this invention is not limited only to a following example.
[反応装置]
図1に示した光触媒反応装置を用いて試験した。図2にUV-LED反応装置系統図を示した。UV-LED照射装置に電源を供給する電源はDC24V、電源容量35W(外部照射型30W、内部照射型5W)とした。UV-LEDランプは光量可変型を用い、消費電流値可変による調整を行った。主電源の他、外部照射装置、内部照射装置個々に電源供給が出来るよう、切り替えスイッチ、電圧計、電流計を装備した。
[Reactor]
The test was carried out using the photocatalytic reaction apparatus shown in FIG. FIG. 2 shows a system diagram of the UV-LED reactor. The power supply for supplying power to the UV-LED irradiation apparatus was DC 24 V, power supply capacity 35 W (external irradiation type 30 W, internal irradiation type 5 W). The UV-LED lamp was a variable light quantity type and was adjusted by changing the current consumption value. In addition to the main power supply, a switch, a voltmeter, and an ammeter were installed to supply power to the external and internal irradiation devices.
流量計16はCO2用フロー式ガス流量計を使用し、循環ポンプ17は循環反応に供するガス循環ポンプを使用した。原料ガスは、反応による容量変化に対応するため10Lテドラーパック18を使用した。 The flow meter 16 was a CO 2 flow type gas flow meter, and the circulation pump 17 was a gas circulation pump used for a circulation reaction. As a raw material gas, a 10 L tedlar pack 18 was used in order to cope with a capacity change due to a reaction.
[反応試験]
容量500mlの反応容器1内に、420mlのイオン交換水と、光触媒Cとして酸化チタン(ルチル型)3.0gを入れた。反応容器1を、超音波スターラー((株)日本精機製作所製のヨウカイくん USS−1)12に適量の水14があることを確認し、UV-LED照射装置へセットした。超音波及びスターラー15を運転して光触媒Cを攪拌し、チラーを運転して冷却用コイル6に冷却水を循環しながら、反応容器内の温度を20℃とした。
[Reaction test]
In a reaction vessel 1 having a capacity of 500 ml, 420 ml of ion-exchanged water and 3.0 g of titanium oxide (rutile type) as a photocatalyst C were placed. The reaction vessel 1 was confirmed to have an appropriate amount of water 14 in an ultrasonic stirrer (Yokai-kun USS-1 manufactured by Nippon Seiki Seisakusho Co., Ltd.) 12 and set in a UV-LED irradiation device. The temperature inside the reaction vessel was set to 20 ° C. while the photocatalyst C was stirred by operating the ultrasonic wave and the stirrer 15 and the cooling water was circulated through the cooling coil 6 by operating the chiller.
テドラーパックに原料ガス(Arガス)を封入し、反応容器内をパージした。次いで、テドラーパックに原料ガス(Arガス)を封入し、反応装置に設置した。循環ポンプ17を運転し循環流量を規定値にセットし、10分以上循環させたら原料ガス組成をガスクロマトグラフィーにて確認した。 A source gas (Ar gas) was sealed in a Tedlar pack, and the inside of the reaction vessel was purged. Next, a raw material gas (Ar gas) was sealed in the Tedlar pack and installed in the reactor. The circulation pump 17 was operated, the circulation flow rate was set to a specified value, and after circulating for 10 minutes or more, the raw material gas composition was confirmed by gas chromatography.
外部照射用UV-LEDの空冷用ポンプを運転し、UV遮蔽保護カバーを設置した。UV-LED照射装置電源をONにし、徐々に電流をかけ、外側のUV出力23.3W、内側のUV出力1.8Wにて紫外線を照射し、反応試験を開始した。規定時間反応させたら、テドラーパック内のガスをガスクロマトグラフィーにて分析した。4時間反応させた後、光触媒分散水をろ過し、水に含まれているガスをガスクロマトグラフィーにて分析した。試験後は速やかに反応容器を洗浄した。 The external cooling UV-LED air cooling pump was operated, and a UV shielding protective cover was installed. The UV-LED irradiator was turned on, a current was gradually applied, and ultraviolet rays were irradiated with an outer UV output of 23.3 W and an inner UV output of 1.8 W, and a reaction test was started. After reacting for a specified time, the gas in the Tedlar pack was analyzed by gas chromatography. After reacting for 4 hours, the photocatalyst-dispersed water was filtered, and the gas contained in the water was analyzed by gas chromatography. After the test, the reaction vessel was immediately washed.
その結果、表1に示す量のH2が発生していた。 As a result, the amount of H 2 shown in Table 1 was generated.
表1の結果から、本発明の光触媒反応装置において、光触媒の作用により水から水素が発生することが確認できたので、CO2化学固定化における触媒反応の評価装置として使用できることが分かった。 From the results of Table 1, since it was confirmed that hydrogen was generated from water by the action of the photocatalyst in the photocatalytic reaction device of the present invention, it was found that it can be used as an evaluation device for catalytic reaction in CO 2 chemical immobilization.
本発明の光触媒反応装置は、非常に簡易な操作で比較的短時間で光触媒反応の評価を実施することが可能であり、CO2の有機物固定反応における化学固定化反応プロセスの評価を始め、各種の光触媒反応の評価に有効である。 The photocatalytic reaction apparatus of the present invention is capable of evaluating a photocatalytic reaction in a relatively short time with a very simple operation, and has been evaluating various chemical immobilization reaction processes in a CO 2 organic substance fixing reaction, It is effective for the evaluation of photocatalytic reactions.
1 反応容器
2 透明樹脂板
3 UV-LED(外部照射用)
4 上部開口容器
5 UV-LED(内部照射用)
6 冷却装置
7 ガス導入口
8 ガス排出口
9 温度計
10 UV−LED用電源配線
11 原料ガスバブリング装置
12 超音波スターラー
13 UV遮蔽保護カバー
14 水
15 スターラー
16 流量計
17 循環ポンプ
18 テドラーパック
1 reaction vessel 2 transparent resin plate 3 UV-LED (for external irradiation)
4 Upper opening container 5 UV-LED (for internal irradiation)
6 Cooling device 7 Gas inlet 8 Gas outlet 9 Thermometer 10 UV-LED power supply wiring 11 Raw material gas bubbling device 12 Ultrasonic stirrer 13 UV shielding protective cover 14 Water 15 Stirrer 16 Flow meter 17 Circulation pump 18 Tedlar pack
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