WO2011067873A1 - 二酸化炭素還元方法、並びに、それに用いる二酸化炭素還元触媒および二酸化炭素還元装置 - Google Patents
二酸化炭素還元方法、並びに、それに用いる二酸化炭素還元触媒および二酸化炭素還元装置 Download PDFInfo
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- WO2011067873A1 WO2011067873A1 PCT/JP2010/003975 JP2010003975W WO2011067873A1 WO 2011067873 A1 WO2011067873 A1 WO 2011067873A1 JP 2010003975 W JP2010003975 W JP 2010003975W WO 2011067873 A1 WO2011067873 A1 WO 2011067873A1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
Definitions
- the present invention relates to a carbon dioxide reduction method, and a carbon dioxide reduction catalyst and a carbon dioxide reduction device used therefor.
- carbon dioxide is a very stable molecule, and conventionally, its electric reduction requires a very large overvoltage.
- catalysts that can reduce this overvoltage.
- Various materials have been studied as catalysts, but no significant effect has been obtained.
- metals (including alloys) and molecular materials also have a durability problem that they deteriorate when used as a catalyst for a long time. For this reason, no catalyst material having practical utility has been found.
- Non-Patent Document 1 copper, cobalt porphyrin (see Non-Patent Document 1), nickel cyclam complex (see Non-Patent Document 2), and the like have been reported as catalysts for reducing carbon dioxide.
- Patent Document 1 a method has also been attempted in which carbon dioxide is reduced by reacting under high temperature and high pressure conditions using hydrogen or the like instead of in a solution.
- Patent Document 2 a reduction reaction of carbon dioxide with alkylbenzene has also been proposed.
- the conventional electrode catalyst material capable of reducing carbon dioxide in a solution as described above has a problem that the overvoltage is still high and the reaction does not easily proceed. Further, the conventional material has a durability problem that it deteriorates due to a long-time catalytic reaction.
- carbon dioxide can be reduced to carbon monoxide, formic acid, methane, etc., and these can be provided at low cost with energy saving. It becomes possible.
- a carbon dioxide reduction technique is very useful as a technique for reducing carbon dioxide.
- the carbon dioxide reduction technology becomes very useful as a resource recycling method with less environmental load by combining with photocatalytic technology and photovoltaic power generation in the future.
- the present invention is a method and apparatus that can reduce carbon dioxide in a solution, and uses a catalyst material that has high durability and can reduce carbon dioxide at an overvoltage lower than that of conventional methods and apparatuses. It is an object to provide a carbon dioxide reduction method and a carbon dioxide reduction device. Another object of the present invention is to provide a carbon dioxide reduction catalyst that can reduce carbon dioxide in a solution, has high durability, and can reduce carbon dioxide at an overvoltage lower than that of a conventional carbon dioxide reduction catalyst. To do.
- the carbon dioxide reduction method of the present invention comprises: A step of contacting an electrode containing a carbide of at least any one element selected from group V elements (vanadium, niobium and tantalum) with an electrolytic solution; Introducing carbon dioxide into the electrolyte, and reducing the introduced carbon dioxide with the electrode; It is a method including.
- the carbon dioxide reduction catalyst of the present invention contains a carbide of at least one element selected from group V elements (vanadium, niobium and tantalum).
- the carbon dioxide reduction device of the present invention is An electrolyte, A tank containing the electrolyte solution; A first electrode disposed in contact with the electrolytic solution and containing a carbide of at least one element selected from group V elements (vanadium, niobium and tantalum); A second electrode disposed in contact with the electrolyte and electrically connected to the first electrode; A solid electrolyte disposed between the first electrode and the second electrode and separating the inside of the tank into a region on the first electrode side and a region on the second electrode side; A gas inlet for introducing carbon dioxide into the electrolyte; It has.
- the carbon dioxide reduction method and the carbon dioxide reduction device of the present invention are a method and an apparatus for reducing carbon dioxide in a solution. Furthermore, the electrode for reducing carbon dioxide (first electrode) has high durability, And the catalyst material which can reduce
- the carbon dioxide reduction catalyst of the present invention can reduce carbon dioxide in a solution, has high durability, and can reduce carbon dioxide with an overvoltage lower than that of a conventional carbon dioxide reduction catalyst.
- FIG. 2A is a diagram showing an adsorption state of carbon dioxide on tantalum carbide by electronic state calculation
- FIG. 2B is a diagram showing an adsorption state of carbon monoxide on tantalum carbide by electronic state calculation
- 2 is an X-ray diffraction pattern showing a crystal structure of tantalum carbide formed on a silicon substrate by sputtering. It is a schematic diagram of the electrochemical cell used for the measurement in an Example.
- the carbon dioxide reduction method and the carbon dioxide reduction apparatus in the present embodiment use the carbon dioxide reduction catalyst of the present invention containing a carbide of at least one element selected from group V elements (vanadium, niobium and tantalum) as an electrode. And a method and apparatus for reducing carbon dioxide in a solution.
- group V elements vanadium, niobium and tantalum
- the carbon dioxide reduction method of the present embodiment includes a step of bringing an electrode containing a carbide of at least one element selected from vanadium, niobium and tantalum into contact with an electrolytic solution, and introducing carbon dioxide into the electrolytic solution. And reducing the introduced carbon dioxide with the electrode.
- An electrode containing a carbide of at least one element selected from vanadium, niobium, and tantalum functions as a working electrode that reduces carbon dioxide.
- a conductive silicon substrate can be used as an electrode substrate, and an electrode obtained by growing tantalum carbide on the conductive silicon substrate by RF (Radio-Frequency) sputtering can be used.
- the electrode substrate at this time is not particularly limited to a conductive silicon substrate as long as it has conductivity.
- Commonly used electrode substrates include a substrate made of an inert metal such as gold and a glassy carbon substrate.
- the method for forming a thin film of tantalum carbide is not limited.
- Such a tantalum carbide thin film is immersed in an electrolytic solution with a working electrode provided on an electrode substrate as a carbon dioxide reduction catalyst and a counter electrode electrically connected to the electrode, and carbon dioxide is introduced into the electrolytic solution. By doing so, carbon dioxide in the electrolytic solution can be reduced by the catalytic activity of tantalum carbide.
- an electrode provided with a thin film of tantalum carbide is used.
- an electrode having powdered tantalum carbide supported on an electrode substrate is not the thin film as described above. Is obtained. Further, as will be described later in Examples, similar reduction of carbon dioxide was confirmed not only by tantalum carbide but also by an electrode sputtered with niobium carbide or vanadium carbide.
- each material is supported by a supporting method so that the catalyst is stably supported or formed on the electrode substrate in the solution. It is desirable to adjust the conditions of the film formation method.
- the carbon dioxide reduction device of the present invention one having the same configuration as the electrochemical cell (see FIG. 4) used in the examples described later can be used. That is, as shown in FIG. 4, the carbon dioxide reduction device of the present embodiment includes an electrolytic solution 47, a tank 48 in which the electrolytic solution 47 is accommodated, an electrolytic solution 47, and a group V element (vanadium).
- the carbon dioxide reduction device of the present embodiment includes an electrolytic solution 47, a tank 48 in which the electrolytic solution 47 is accommodated, an electrolytic solution 47, and a group V element (vanadium).
- the working electrode 41 and the counter electrode 43 are completely immersed in the electrolytic solution 47.
- the present invention is not limited to this, and the working electrode 41 and the counter electrode 43 are in contact with the electrolytic solution 47. It only has to be arranged.
- the electrochemical cell shown in FIG. 4 was used for the measurement in the Example, it is a three-electrode cell further provided with a reference electrode 42, but when used as a carbon dioxide reduction device Since the measurement of potential is not essential, the reference electrode 42 is not necessarily provided.
- an electrode in which a tantalum carbide thin film was formed on a conductive silicon substrate was prepared, and as a result of analyzing a substance generated when carbon dioxide was reduced by this electrode, the product was analyzed. It was confirmed that carbon monoxide, formic acid, methane and ethanol were produced.
- a gas chromatograph was used for analysis of gas components, and a liquid chromatograph was used for analysis of liquid components.
- FIG. 1 shows the adsorption energy of carbon dioxide (CO 2 ) on the (001) plane of tantalum carbide (TaC) and the dioxide dioxide on the (001) plane of niobium carbide (NbC) by calculating the electronic state using density functional theory A comparison with the adsorption energy of carbon (CO 2 ) is shown (CO 2 adsorption in the upper right of FIG. 1).
- a catalytic reaction requires a small adsorption energy.
- the energy required for CO adsorption is reported to be ⁇ 0.62 eV (B. Hammer et al., Phys. Rev. Lett, 76 2141 (1996)).
- the greater the adsorption energy the less likely the catalytic reaction will occur. This is because the greater the adsorption energy, the stronger the adsorption and the less likely the catalytic reaction occurs.
- the adsorption energy per ⁇ 6 eV is shown for CO. Therefore, when single metal tantalum or niobium is used as an electrode, since the adsorption of CO is too strong, no catalytic reaction is shown.
- CO 2 is adsorbed on the solid surface of the electrode (carbon dioxide reduction catalyst provided on the electrode; hereinafter referred to as catalyst), and then this CO 2 is reduced by protons to become CO.
- catalyst carbon dioxide reduction catalyst provided on the electrode
- the stable structure for example, structure as shown to FIG. 2A which the carbon dioxide adsorb
- carbon dioxide reduction it is known that a large overvoltage is required in a process in which one electron is transferred to carbon dioxide molecules and adsorbed on the catalyst surface.
- FIG. 2A the adsorption state of carbon dioxide on the catalyst surface (TaC (001) plane) described above is shown in FIG. 2A, and the adsorption state of carbon monoxide is shown in FIG. 2B.
- the adsorption state diagrams shown in FIGS. 2A and 2B are obtained by calculation.
- the numbers in the figure indicate the distance from the surface element in the stable structure.
- the distance between TaC and CO 2 adsorbed on TaC is 2.486 mm.
- FIG. 2B the distance between TaC and CO adsorbed on TaC is 2.164 mm. These distances are larger than the distance between C and O in carbon monoxide (about 1.1 cm). This reflects that the adsorption of TaC and CO 2 and the adsorption of TaC and CO are shallow.
- the carbon dioxide reduction method and the carbon dioxide reduction device of the present embodiment unlike the gas phase reduction reaction performed in a high-pressure and high-temperature environment, the reduction reaction using only a direct current from a DC power source at normal temperature and pressure. Is possible. As a more environmentally friendly method and apparatus configuration, a method using a solar cell as an external power source, or a reduction catalyst using solar energy by combination with a photocatalyst is possible.
- the carbon dioxide reduction method and the carbon dioxide reduction device according to the present embodiment are extremely promising technologies as energy-saving carbon dioxide countermeasures in homes and regions where so-called large-scale facilities cannot be introduced.
- vanadium carbide, niobium carbide, and tantalum carbide are used as the carbon dioxide reduction catalyst. What is necessary is just the material containing the carbide
- the reduction reaction of carbon dioxide using the carbon dioxide reduction catalyst of the present invention can be carried out, for example, by blowing carbon dioxide into an electrolytic solution that is a liquid composition or by introducing carbon dioxide through a circulation system. It can be implemented as.
- the following examples illustrate the present invention in more detail.
- Example 1 First, a 1 cm square conductive silicon substrate was prepared as an electrode substrate. The chamber was evacuated to 1.0 ⁇ 10 ⁇ 4 Pa with a pump and then introduced with argon gas. By sputtering at an output of 100 W in an argon gas atmosphere of 1.0 ⁇ 10 ⁇ 1 Pa, tantalum carbide was formed on the electrode substrate with a thickness of about 3000 mm. The crystal structure of tantalum carbide was evaluated by X-ray diffraction. The diffraction pattern at this time is shown in FIG. As shown by arrows in FIG. 3, a crystal structure peak of tantalum carbide having a sodium chloride structure was confirmed in the diffraction pattern.
- the formed tantalum carbide is in a polycrystalline state in which several plane indices appear, but a crystalline thin film is formed on a silicon substrate (electrode substrate). confirmed.
- FIG. 4 shows a schematic diagram of the electrochemical cell used for the measurement in this example.
- the electrochemical cell used in this example was a triode cell having a working electrode 41, a reference electrode 42, and a counter electrode 43, and a potentiostat 44 was provided.
- the electrolytic solution 47 was accommodated in the tank 48, and the electrodes 41 to 43 were disposed in a state immersed in the electrolytic solution 47.
- a solid electrolyte membrane 45 is provided between the working electrode 41 and the counter electrode 43 so as to be immersed in the electrolytic solution 47.
- the solid electrolyte membrane 45 allows the inside of the tank 48 to be on the working electrode 41 side. It was separated into a region and a region on the counter electrode 43 side.
- This electrochemical cell was provided with a gas inlet 46 for introducing carbon dioxide into the electrolytic solution 47.
- the working electrode 41 used was the electrode prepared in this example
- the reference electrode 42 was a silver / silver chloride electrode
- the counter electrode 43 was a platinum electrode.
- the triode cell was evaluated by sweeping the potential with a potentiostat 44.
- As the electrolytic solution 47 0.1M (0.1 mol / L) potassium hydrogen carbonate was used.
- the solid electrolyte membrane 45 that partitions the working electrode 41 and the counter electrode 43 also had a function of preventing mixing of generated gas components. Carbon dioxide was introduced into the cell via the gas introduction pipe 46 and bubbled into an electrolytic solution 47 of potassium hydrogen carbonate.
- FID gas chromatograph gas chromatograph
- FID gas chromatograph flame ion detector
- a liquid chromatograph was used for analysis of the liquid component. The measurement result which confirmed the production
- generation of carbon monoxide using the FID gas chromatograph using the separation column of Porapak N is shown in FIG. In this case as well, it is programmed to detect carbon monoxide around 2.5 min and methane around 6.5 min after the start of measurement by controlling the valve with a preset time sequence. It was. As a result, as shown in FIG. 8, since voltage peak values were observed around 2.5 and 6.5 min, it was confirmed that carbon monoxide and methane were produced.
- FIG. 9 shows the measurement results confirming the formation of formic acid by liquid chromatography.
- a voltage peak was confirmed around this time. This confirmed that formic acid was produced.
- a group V element carbon compound such as tantalum carbide when used as a carbon dioxide reduction catalyst, carbon dioxide is reduced to produce carbon monoxide, formic acid, methane, ethylene, and ethane as products. Indicated. As described in the embodiment, it is considered that a carbon compound of a group V element such as tantalum carbide can reduce carbon dioxide with an overvoltage lower than that of a conventional carbon dioxide reduction catalyst. Further, tantalum carbide, niobium carbide, and vanadium carbide are generally compounds that have higher durability in solution than single metals and metal complexes. Therefore, it can be said that the carbon dioxide reduction catalyst of the present invention has high durability and can reduce carbon dioxide at an overvoltage lower than that of the conventional carbon dioxide reduction catalyst.
- the present invention has demonstrated the reduction of carbon dioxide at a lower overvoltage in a highly durable compound of a group V element carbon compound.
- Carbon dioxide is reduced to carbon monoxide, formic acid, methane, etc. Not only can it be provided at low cost with low energy, it can also be used as a technology to reduce carbon dioxide.
Abstract
Description
V族元素(バナジウム、ニオブおよびタンタル)から選ばれる少なくとも何れか1種の元素の炭化物を含有する電極を電解液に接触させる工程と、
前記電解液に二酸化炭素を導入し、導入された前記二酸化炭素を前記電極によって還元する工程と、
を含む方法である。
電解液と、
前記電解液が収容された槽と、
前記電解液と接して配置され、かつV族元素(バナジウム、ニオブおよびタンタル)から選ばれる少なくとも何れか1種の元素の炭化物を含有する第1電極と、
前記電解液と接して配置され、かつ前記第1電極と電気的に接続された第2電極と、
前記第1電極と前記第2電極との間に配置され、前記槽内を、前記第1電極側の領域と前記第2電極側の領域とに分離する、固体電解質と、
前記電解液に二酸化炭素を導入するガス導入口と、
を備えている。
まず、電極基板として、1cm角の導電性シリコン基板を用意した。チャンバー内を1.0×10-4Paまでポンプで真空にした後にアルゴンガスを導入した。1.0×10-1Paのアルゴンガス雰囲気中で100Wの出力でスパッタリングすることにより、炭化タンタルを電極基板上に厚さ約3000Åで成膜した。炭化タンタルの結晶構造をX線回折で評価した。このときの回折パターンを、図3に示す。図3中に矢印で示すように、回折パターンに、塩化ナトリウム構造の炭化タンタルの結晶構造ピークが確認された。
比較のため、炭素を触媒として用いて、二酸化炭素還元の様子を調べた。カーボンペーパーで形成した電極を準備し、これを作用電極として用いた点以外は、実施例1と同様の方法で電解反応を行った。その結果、CO2還元による還元電流は観測されず、炭素はCO2還元に対して不活性であり、電解反応による生成物は水素(H2)のみであった。
比較のため、V族元素以外の金属元素の炭化物を触媒として用いて、二酸化炭素還元の様子を調べた。チタニウム(Ti)、モリブデン(Mo)などの炭化物粒子を作製し、それぞれの炭化物粒子をカーボンペーパーに担持して、作用電極とした。これ以外は、実施例1と同様の方法で電解反応を行った。その結果、基材として用いたカーボンペーパーと同様の特性を示し、H2のみが生成され、CO、炭化水素、HCOOHなどの生成物は得られなかった。
Claims (3)
- V族元素(バナジウム、ニオブおよびタンタル)から選ばれる少なくとも何れか1種の元素の炭化物を含有する電極を電解液に接触させる工程と、
前記電解液に二酸化炭素を導入し、導入された前記二酸化炭素を前記電極によって還元する工程と、
を含む、二酸化炭素還元方法。 - V族元素(バナジウム、ニオブおよびタンタル)から選ばれる少なくとも何れか1種の元素の炭化物を含有する、二酸化炭素還元触媒。
- 電解液と、
前記電解液が収容された槽と、
前記電解液と接して配置され、かつV族元素(バナジウム、ニオブおよびタンタル)から選ばれる少なくとも何れか1種の元素の炭化物を含有する第1電極と、
前記電解液と接して配置され、かつ前記第1電極と電気的に接続された第2電極と、
前記第1電極と前記第2電極との間に配置され、前記槽内を、前記第1電極側の領域と前記第2電極側の領域とに分離する、固体電解質と、
前記電解液に二酸化炭素を導入するガス導入口と、
を備えた、二酸化炭素還元装置。
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CN2010800100508A CN102341529A (zh) | 2009-12-04 | 2010-06-15 | 二氧化碳还原方法、及在其中使用的二氧化碳还原催化剂和二氧化碳还原装置 |
US13/190,975 US20120018311A1 (en) | 2009-12-04 | 2011-07-26 | Carbon dioxide reduction method, and carbon dioxide reduction catalyst and carbon dioxide reduction device used for the method |
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JP2019203163A (ja) * | 2018-05-22 | 2019-11-28 | 日本電信電話株式会社 | 電解還元装置及び電解還元方法 |
WO2020005483A1 (en) * | 2018-06-29 | 2020-01-02 | Illinois Institute Of Technology | Artificial leaf-based facade cladding system for energy production and carbon sequestration |
WO2020005482A1 (en) * | 2018-06-29 | 2020-01-02 | Illinois Institute Of Technology | Transition metal mxene catalysts for conversion of carbon dioxide to hydrocarbons |
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JP2004176129A (ja) * | 2002-11-27 | 2004-06-24 | Kotaro Ogura | 二酸化炭素からのエチレンの選択的製造方法 |
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JP2011140719A (ja) | 2011-07-21 |
JP5386533B2 (ja) | 2014-01-15 |
US20120018311A1 (en) | 2012-01-26 |
CN102341529A (zh) | 2012-02-01 |
JPWO2011067873A1 (ja) | 2013-04-18 |
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