JP6216194B2 - Ammonia synthesis method by thermochemical cycle - Google Patents
Ammonia synthesis method by thermochemical cycle Download PDFInfo
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本発明は新規なアンモニアの合成方法に関し、特に、化石燃料を原料とすることなく、空気と水からアンモニアを合成する方法に関する。 The present invention relates to a novel method for synthesizing ammonia, and more particularly to a method for synthesizing ammonia from air and water without using fossil fuel as a raw material.
アンモニアは、窒素と水素から合成するハーバー・ボッシュ法によって合成されており、現在重要な肥料の一つとなっている。しかしながら上記の合成方法は、原料水素を化石燃料から製造しているため、化石燃料の枯渇が懸念される現在、化石燃料を使用しない新たな方法が望まれるに至った。またアンモニアには、環境負荷の小さい水素に対する、安全なキャリアガスとしての需要も高まっているため、今後アンモニアの需要は、現状より更に高まるものと予想される。 Ammonia is synthesized by the Harbor Bosch method, which is synthesized from nitrogen and hydrogen, and is currently one of the important fertilizers. However, since the above synthesis method produces raw material hydrogen from fossil fuels, a new method that does not use fossil fuels has been desired at present when there is concern about the depletion of fossil fuels. In addition, demand for ammonia as a safe carrier gas for hydrogen, which has a low environmental burden, is expected to increase further in the future.
原料水素を化石燃料に依存しない新たな方法としては、窒素とハロゲン化水素とを反応させた後、得られたハロゲン化アンモニウムを分解してアンモニアを得ることを特徴とするアンモニアの合成方法が既に知られている（特許文献１）。しかしながらこの方法は、ハロゲン化水素という特殊な原料を使用するために、作業性が悪いだけでなく環境負荷を悪化させ、また、装置の腐食防止も必要となるため、製造コスト的にも有利な方法ではないという欠点があった。 As a new method that does not depend on fossil fuel for raw material hydrogen, there is already an ammonia synthesis method characterized by reacting nitrogen and hydrogen halide and then decomposing the obtained ammonium halide to obtain ammonia. Known (Patent Document 1). However, since this method uses a special raw material such as hydrogen halide, not only the workability is bad, but also the environmental load is deteriorated, and it is also necessary to prevent the corrosion of the apparatus. There was a drawback that it was not a method.
上記の欠点は、（１）窒素ガスと炭酸ガスをプラズマ反応させて一酸化窒素と一酸化炭素を生成する第1反応、（２）プラズマ反応によって、炭酸ガスから一酸化炭素と酸素を得る第２反応、及び（３）触媒反応によって、水分子と、得られた一酸化窒素及び一酸化炭素を反応させてアンモニアと炭酸ガスを製造する方法によって大きく改善された（非特許文献１）。本発明者等は、上記の方法について更に検討した結果、炭酸ガスからプラズマ放電反応によって一酸化炭素と酸素を得、得られた一酸化炭素に水分子と窒素分子を加え、これを熱化学触媒反応させた場合には、化石燃料を原料とすることなく、二酸化炭素、水及び窒素ガスを原料ガスとして用い、２段階反応でアンモニアガスを製造することができることを見出し本発明に到達した。 The above disadvantages are as follows: (1) a first reaction in which nitrogen gas and carbon dioxide gas are reacted to generate nitrogen monoxide and carbon monoxide; and (2) carbon monoxide and oxygen are obtained from carbon dioxide gas by plasma reaction. This was greatly improved by a method of producing ammonia and carbon dioxide gas by reacting water molecules with the obtained nitrogen monoxide and carbon monoxide by two reactions and (3) catalytic reaction (Non-patent Document 1). As a result of further study on the above method, the present inventors obtained carbon monoxide and oxygen from carbon dioxide gas by a plasma discharge reaction, added water molecules and nitrogen molecules to the obtained carbon monoxide, and obtained the thermochemical catalyst. In the case of reaction, the present inventors have found that ammonia gas can be produced by a two-stage reaction using carbon dioxide, water and nitrogen gas as raw material gas without using fossil fuel as raw material.
したがって本発明の第1の目的は、化石燃料を原料とすることなくアンモニアガスを製造する方法を提供することにある。
本発明の第２の目的は、一酸化炭素、水及び窒素ガスを原料とし、アンモニアを合成することのできる熱化学触媒を提供することにある。
本発明の第３の目的は、化石燃料を原料として使用しないだけでなくエネルギー源としても使用することのない、アンモニア合成方法を提供することにある。
Accordingly, a first object of the present invention is to provide a method for producing ammonia gas without using fossil fuel as a raw material.
The second object of the present invention is to provide a thermochemical catalyst capable of synthesizing ammonia using carbon monoxide, water and nitrogen gas as raw materials.
A third object of the present invention is to provide an ammonia synthesis method that does not use fossil fuel as a raw material but also as an energy source.
本発明の上記の諸目的は、下記式（１）の放電反応によって、炭酸ガスを分解して一酸化炭素を製造し、次いで、水分子、窒素ガス及び上記式（１）によって得られた一酸化炭素を原料とし、Pt、Ru、及びFeの中から選択された少なくとも1種の触媒を用いて、下記式（２）で表される熱化学触媒反応によってアンモニアを製造する方法；
1.5CO2 → 1.5CO ＋ 0.75O2 （１）
1.5H2O ＋ 0.5N2 ＋ 1.5CO → NH3 ＋ 1.5CO2 （２）
本発明においては、上記（１）式の放電反応を、室温〜２００℃の条件下で実施することが好ましく、式（２）の触媒反応を室温〜５００℃の条件下で実施することが好ましい。
また、放電反応の電源を、自然エネルギーを用いた発電システムによって賄うことが好ましい。
The above objects of the present invention are to produce carbon monoxide by decomposing carbon dioxide gas by the discharge reaction of the following formula (1), and then obtain water molecules, nitrogen gas, and one obtained by the above formula (1). A method for producing ammonia by a thermochemical catalytic reaction represented by the following formula (2) using carbon oxide as a raw material and using at least one catalyst selected from Pt, Ru, and Fe;
1.5CO 2 → 1.5CO + 0.75O 2 (1)
1.5H 2 O + 0.5N 2 + 1.5CO → NH 3 + 1.5CO 2 (2)
In the present invention, the discharge reaction of the above formula (1) is preferably carried out under conditions of room temperature to 200 ° C., and the catalytic reaction of formula (2) is preferably carried out under conditions of room temperature to 500 ° C. .
Moreover, it is preferable that the power source of the discharge reaction is provided by a power generation system using natural energy.
本発明のアンモニア合成方法は化石燃料を原料としないので、化石燃料の消費抑制に貢献するだけでなく、作業性及び環境保全の観点からも優れているので、将来のアンモニア合成法として有望である。 Since the ammonia synthesis method of the present invention does not use fossil fuel as a raw material, it not only contributes to the suppression of fossil fuel consumption, but is also excellent from the viewpoint of workability and environmental conservation, and is therefore promising as a future ammonia synthesis method. .
以下、本発明を詳細に説明するが、本発明はこれらによって限定されるものではなく、当業者であれば本願明細書の記載に基づいて容易に設計変更して実施することが出来る発明を包含することは当然である。 Hereinafter, the present invention will be described in detail, but the present invention is not limited thereto, and includes those that can be easily modified and implemented by those skilled in the art based on the description of the present specification. It is natural to do.
下記式（１）で表される放電反応は、室温〜２００℃の炭酸ガスを、印可電圧8〜10kVで、約1mmの距離を設けた電極間に、安定な放電が可能となる圧力である約1atmとなるように約1L/minの流速で流すことによって容易に行うことができる。なお、マイクロ波キャビティを用いてマイクロ波放電を行わせる事も可能である。
1.5CO2 → 1.5CO ＋ 0.75O2 （１）
本発明においては、2つの電極間に純度99%以上、厚さ約2.5mmのアルミナ板を誘電体として挟み込み、陽極と前記アルミナ板の間に約1mmの間隔を設け、該間隔によって形成された空間内で放電反応を行わせることが好ましい。また、陰極側の電極にはアルミニウム板を使用することが好ましい。陽極側の電極としては、約1mmのアルミニウム3003の板に、下記１〜４の処理を行って調整したアルマイト電極を使用することが特に好ましい。
１．処理を施したい場所以外をマスキング材で覆う。
２．約20質量%の水酸化ナトリウム溶液に約3分、約30質量%の硝酸溶液に約1分浸して前処理する。
３．被処理アルミニウムを陽極とし、約50A/m2の電流を流した約4質量%のシュウ酸水溶液に約16時間浸して陽極酸化処理する。
４．マスキング材を剥がし、空気中約350℃にて約1時間焼成する。
The discharge reaction represented by the following formula (1) is a pressure at which stable discharge is possible between electrodes having a distance of about 1 mm at an applied voltage of 8 to 10 kV with carbon dioxide at room temperature to 200 ° C. It can be easily performed by flowing at a flow rate of about 1 L / min so as to be about 1 atm. It is also possible to cause microwave discharge using a microwave cavity.
1.5CO 2 → 1.5CO + 0.75O 2 (1)
In the present invention, an alumina plate having a purity of 99% or more and a thickness of about 2.5 mm is sandwiched between the two electrodes as a dielectric, and an interval of about 1 mm is provided between the anode and the alumina plate, and the space formed by the interval is formed. It is preferable to cause a discharge reaction. Moreover, it is preferable to use an aluminum plate for the electrode on the cathode side. As the anode-side electrode, it is particularly preferable to use an alumite electrode prepared by performing the following treatments 1 to 4 on a plate of about 300 mm of aluminum 3003.
1. Cover the areas other than where you want to treat with masking material.
2. Pretreatment is performed by immersing in about 20% by mass sodium hydroxide solution for about 3 minutes and about 30% by mass in nitric acid solution for about 1 minute.
3. Anodizing is performed by immersing in an aqueous solution of about 4% by mass of oxalic acid at an electric current of about 50 A / m 2 for about 16 hours using aluminum to be treated as an anode.
4). Peel off the masking material and bake in air at about 350 ° C for about 1 hour.
本発明においては、前記した放電反応によって一酸化炭素が生成した下流側に、水分子及び窒素ガスを添加し、Pt、Ru、及びFe等の中から選択された少なくとも1種の触媒が充填された熱化学触媒反応管を通して、下記式（２）で表される熱化学触媒反応を実施し、アンモニアを製造する。本発明においては、生産効率の観点から特にPtを使用することが好ましい。
1.5H2O ＋ 0.5N2 ＋ 1.5CO → NH3 ＋ 1.5CO2 （２）
熱化学触媒反応管を通過した反応ガスを水に通せば、炭酸アンモニウム水溶液として容易に、生成したアンモニアを取り出すことができるが、本発明はこの方法に限定されるものではない。
In the present invention, water molecules and nitrogen gas are added to the downstream side where carbon monoxide is generated by the above-described discharge reaction, and at least one catalyst selected from Pt, Ru, Fe, and the like is filled. Through the thermochemical catalyst reaction tube, the thermochemical catalyst reaction represented by the following formula (2) is carried out to produce ammonia. In the present invention, it is particularly preferable to use Pt from the viewpoint of production efficiency.
1.5H 2 O + 0.5N 2 + 1.5CO → NH 3 + 1.5CO 2 (2)
If the reaction gas that has passed through the thermochemical catalyst reaction tube is passed through water, the produced ammonia can be easily taken out as an aqueous ammonium carbonate solution, but the present invention is not limited to this method.
前記式（２）の反応で使用する触媒は、触媒金属（白金、ルテニウム、鉄など）の硝酸塩水溶液を、活性炭やアルミナ粉末等の担体に含侵させ、乾燥空気によって乾燥し、水分が少なくなった時点で、約80℃の乾燥機に入れて約12時間乾燥した後、約2時間水素還元して得ることができる。本発明においては、得られた粉末状の触媒を反応管に充填して使用する。なお、担体に担持された各触媒の金属割合は、白金が約5質量%、ルテニウムが約1質量%、鉄は約10質量%であることが好ましい。 The catalyst used in the reaction of the formula (2) impregnates an aqueous nitrate solution of a catalytic metal (platinum, ruthenium, iron, etc.) with a support such as activated carbon or alumina powder, and is dried with dry air, so that the water content is reduced. In this case, it can be obtained by placing in a dryer at about 80 ° C. for about 12 hours and then reducing with hydrogen for about 2 hours. In the present invention, the obtained powdered catalyst is used by filling a reaction tube. The metal ratio of each catalyst supported on the carrier is preferably about 5 mass% for platinum, about 1 mass% for ruthenium, and about 10 mass% for iron.
前記式（２）の反応で使用する触媒反応管は、例えば、ステンレス管に触媒を緩く充填した後、入口側及び出口側にガスが通過できる程度に石英ウールを詰めることによって、容易に調製することができる。また、反応温度は、熱電対を反応管に差し込むことによって容易に測定することができる。 The catalyst reaction tube used in the reaction of the above formula (2) is easily prepared by, for example, filling a stainless steel tube loosely with a catalyst and then filling quartz wool so that gas can pass through the inlet side and the outlet side. be able to. The reaction temperature can be easily measured by inserting a thermocouple into the reaction tube.
ところで、前記式（１）で生成されたCOの殆どは、下記式（３）で表されるシスト反応によって消費され、式（２）の反応に有効に使用される量は少ない。
H2O ＋ CO → CO2 ＋ H2 （３）
しかしながら、２００℃の反応におけるCO１モル当たりの自由エネルギーの変化は、式（２）では-２０kJ、式（３）では-２１kJであり、両者は殆ど同じであるので、触媒を選択することにより、式（２）の反応を主反応にすることができる筈である。
以下本発明を実施例によって更に詳述するが、本発明はこれによって限定されるものではない。
By the way, most of the CO produced by the formula (1) is consumed by the cyst reaction represented by the following formula (3), and the amount effectively used for the reaction of the formula (2) is small.
H 2 O + CO → CO 2 + H 2 (3)
However, the change in free energy per mole of CO in the reaction at 200 ° C. is −20 kJ in the formula (2) and −21 kJ in the formula (3), and both are almost the same. It should be possible to make the reaction of formula (2) the main reaction.
Hereinafter, the present invention will be described in more detail by way of examples, but the present invention is not limited thereto.
＜式（２）の反応用Pt触媒の調製＞
6.6％の硝酸白金水溶液を担体であるアルミナ粉末5ｇに含侵させ、乾燥空気によって乾燥し、水分が少なくなった時点で、80℃の乾燥機中で12時間乾燥し、その後2時間水素還元して5.25ｇの触媒を得た。触媒の担持量は0.25gであった。得られた触媒5.25ｇのうち、約2.39gを後記するステンレス製の反応管に充填した。
＜式（１）反応の実施＞
表面に誘電体層としてアルミナの層を設け、接地した陰極と、前記誘電体層との間隔が1mmとなるように配したアルマイト陽極を内部に有する放電室の前記電極間に8〜10キロボルトのパルス電圧を印可すると共に、内部温度が200℃となるように加熱し、静圧が1atmとなるようにCO2を入口から導入した。この時の流量は1L/分であり、一酸化炭素の収率は5.5%であった。なお、この時の流速は、後記する、後段の熱化学触媒反応器を通過するガスの流速以下である。
<Preparation of Pt catalyst for reaction of formula (2)>
Impregnating 5g of alumina powder as a carrier with 5g of platinum powder as a carrier, drying with dry air, when moisture is low, drying in an oven at 80 ° C for 12 hours, then reducing with hydrogen for 2 hours 5.25 g of catalyst was obtained. The amount of catalyst supported was 0.25 g. About 2.39 g of the obtained catalyst 5.25 g was filled in a stainless steel reaction tube described later.
<Implementation of Formula (1) Reaction>
An alumina layer is provided as a dielectric layer on the surface, and 8 to 10 kilovolts between the electrodes of the discharge chamber having an alumite anode arranged so that the distance between the grounded cathode and the dielectric layer is 1 mm. While applying a pulse voltage, heating was performed so that the internal temperature was 200 ° C., and CO 2 was introduced from the inlet so that the static pressure was 1 atm. The flow rate at this time was 1 L / min, and the yield of carbon monoxide was 5.5%. The flow rate at this time is equal to or lower than the flow rate of the gas passing through the later-stage thermochemical catalyst reactor, which will be described later.
＜式（２）熱化学触媒反応の実施＞
予め調製した前記Pt触媒2.39ｇを、直径7mmで、長さが22.6cmの石英管に充填した反応器を用意した。この反応器を予め２００℃に加熱し、上記放電室の出口から排出されたガスに、N2、CO、H2Oがそれぞれ51.0％9.36％8.41％（残りはAr)となるように水蒸気及び窒素ガスを添加したガスを導入した。この時の全体の流量は168.09ｍｌ/分（4219.83ｍL/g.時間)であった。
反応器を通過したガスを分割採取し、分光光度計（（株）日本分光製のV-530）にかけたところ、NOの生成は確認されず、アンモニアの生成が確認された。
また、反応器を通過したガスを濃度0.1mol/Lの硫酸水溶液中に３０分間バブリングさせ、インドフェノール法によって定量したところ、式（１）反応で生成したCOの約３％が式（２）反応に寄与し、式（２）反応によるアンモニア生成の選択率は約２％であることが確認された。
<Implementation of formula (2) thermochemical catalytic reaction>
A reactor in which 2.39 g of the previously prepared Pt catalyst was packed in a quartz tube having a diameter of 7 mm and a length of 22.6 cm was prepared. This reactor was heated to 200 ° C. in advance, and the gas discharged from the outlet of the discharge chamber was steam and water so that N 2 , CO, and H 2 O would be 51.0% 9.36% 8.41% (remaining Ar), respectively. A gas added with nitrogen gas was introduced. The total flow rate at this time was 168.09 ml / min (4219.83 mL / g. Hour).
When the gas that passed through the reactor was divided and collected and subjected to a spectrophotometer (V-530 manufactured by JASCO Corporation), the production of NO was not confirmed, and the production of ammonia was confirmed.
In addition, the gas that passed through the reactor was bubbled into a 0.1 mol / L sulfuric acid aqueous solution for 30 minutes and quantified by the indophenol method. As a result, about 3% of the CO produced by the reaction of the formula (1) was expressed by the formula (2). Contributing to the reaction, it was confirmed that the selectivity for ammonia production by the reaction of formula (2) was about 2%.
実施例１で使用したPtの代りに、下記のようにして調製したRu触媒を使用したこと以外は実施例１と同様にしてアンモニアを合成した。
＜Ru触媒の調製＞
1.7％の硝酸ルテニウム水溶液を担体である活性炭5ｇに含侵させ、乾燥空気を用いて乾燥し、水分が少なくなった時点で、80℃の乾燥機中で12時間乾燥した後、2時間水素還元して5.05ｇの触媒を得た。触媒の担持量は0.05であった。得られた触媒5.05ｇのうち、約2.39gを実施例1で使用したものと同様の、ステンレス製の反応管に充填した。
アンモニア合成実験の条件は、実質的に実施例１及び３と同じである。
Instead of Pt used in Example 1, ammonia was synthesized in the same manner as in Example 1 except that a Ru catalyst prepared as follows was used.
<Preparation of Ru catalyst>
Impregnate 1.7 g of ruthenium nitrate aqueous solution into 5 g of activated carbon as a carrier, dry it with dry air, and when the water is low, dry in an oven at 80 ° C for 12 hours and then reduce with hydrogen for 2 hours As a result, 5.05 g of a catalyst was obtained. The supported amount of catalyst was 0.05. Of the obtained catalyst (5.05 g), about 2.39 g was charged into a stainless steel reaction tube similar to that used in Example 1.
The conditions for the ammonia synthesis experiment were substantially the same as in Examples 1 and 3.
実施例２で使用したRuの代りに、下記のようにして調製したFe触媒を使用したこと以外は実施例１と同様にしてアンモニアを合成した。
＜Fe触媒の調製＞
19％の硝酸鉄水溶液8mLを担体である活性炭5ｇに含侵させ、乾燥空気を用いて乾燥し、水分が少なくなった時点で80℃の乾燥機中で12時間乾燥した後、2時間水素還元して5.5ｇの触媒を得た。触媒の担持量は0.5gであった。得られた触媒5.5ｇのうち、約2.39gを実施例1で使用したものと同様の、ステンレス製の反応管に充填した。
Ammonia was synthesized in the same manner as in Example 1 except that instead of Ru used in Example 2, an Fe catalyst prepared as described below was used.
<Preparation of Fe catalyst>
Impregnated 8 mL of 19% iron nitrate aqueous solution with 5 g of activated carbon as a carrier, dried using dry air, dried for 12 hours in a dryer at 80 ° C. when the water content was reduced, and then reduced to hydrogen for 2 hours As a result, 5.5 g of catalyst was obtained. The amount of catalyst supported was 0.5 g. Of the 5.5 g of the catalyst obtained, about 2.39 g was charged into a stainless steel reaction tube similar to that used in Example 1.
実施例２及び３における、式（２）反応の実験条件は表１の通りである。
上記の結果から明らかなように、化石燃料を使用することなく、２段反応でアンモニアの合成が可能であることが実証された。収率は、触媒の選択によって改善されるものと予測される。
As is clear from the above results, it was demonstrated that ammonia can be synthesized in a two-stage reaction without using fossil fuel. Yields are expected to be improved by catalyst selection.
本願発明によれば、化石燃料を使用することなく、２段反応でアンモニアの合成が可能であるだけでなく、放電反応のための電源として、太陽発電、風力発電、地熱発電等の自然エネルギーを用いた発電システムを採用する事もできるので、本発明は枯渇が懸念される将来におけるアンモニア合成に大いなる希望をもたらすものであり、産業上極めて重要である。
According to the present invention, it is possible not only to synthesize ammonia in a two-stage reaction without using fossil fuel, but also to use natural energy such as solar power generation, wind power generation, geothermal power generation as a power source for discharge reaction. Since the power generation system used can also be adopted, the present invention brings great hope to ammonia synthesis in the future where there is a concern about depletion, and is extremely important in industry.
Claims (4)
1.5CO2 → 1.5CO ＋ 0.75O2 （１）
1.5H2O ＋ 0.5N2 ＋ 1.5CO → NH3 ＋ 1.5CO2 （２） Carbon dioxide is decomposed by the discharge reaction of the following formula (1) to produce carbon monoxide, and then water molecules, nitrogen gas and carbon monoxide obtained by the above formula (1) are used as raw materials, and Pt, Ru And a method of producing ammonia by a thermochemical catalytic reaction represented by the following formula (2) using at least one catalyst selected from Fe:
1.5CO 2 → 1.5CO + 0.75O 2 (1)
1.5H 2 O + 0.5N 2 + 1.5CO → NH 3 + 1.5CO 2 (2)
The method for producing ammonia according to any one of claims 1 to 3, wherein a power source for a discharge reaction is provided by a power generation system using natural energy.
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