JP2000176284A - Production of ammonia synthesis catalyst and catalyst obtained by the same - Google Patents
Production of ammonia synthesis catalyst and catalyst obtained by the sameInfo
- Publication number
- JP2000176284A JP2000176284A JP10357217A JP35721798A JP2000176284A JP 2000176284 A JP2000176284 A JP 2000176284A JP 10357217 A JP10357217 A JP 10357217A JP 35721798 A JP35721798 A JP 35721798A JP 2000176284 A JP2000176284 A JP 2000176284A
- Authority
- JP
- Japan
- Prior art keywords
- activated carbon
- ammonia synthesis
- synthesis catalyst
- ruthenium
- producing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Catalysts (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、工業的に操作し易
いアンモニア合成触媒の製造方法および同方法で得られ
た触媒に関するものである。The present invention relates to a method for producing an ammonia synthesis catalyst which is easy to operate industrially, and a catalyst obtained by the method.
【０００２】[0002]
【従来の技術】活性炭を触媒担体としてこれにルテニウ
ムのような貴金属を担持したアンモニア合成触媒におい
て、高活性を得るためには同触媒を水素気流下、８５０
℃以上の高温で２４時間以上処理して活性炭中の官能基
を除去する必要がある（特公昭５９−１６８１６号公報
参照）。2. Description of the Related Art In order to obtain high activity in an ammonia synthesis catalyst in which activated carbon is used as a catalyst carrier and a noble metal such as ruthenium is supported thereon, the catalyst is subjected to 850 flow of hydrogen in a stream of hydrogen.
It is necessary to remove the functional groups in the activated carbon by treating at a high temperature of at least ℃ for at least 24 hours (see Japanese Patent Publication No. 59-16816).
【０００３】[0003]
【発明が解決しようとする課題】しかし、水素気流下、
８５０℃以上、２４時間以上という過酷な処理条件で触
媒に処理を施すには、安全対策を施した設備および処理
中の監視のための人員が必要であり、触媒製造のコスト
高を招く要因となる。また、高温で水素を扱うのははな
はだ危険な作業である。However, under a hydrogen stream,
In order to treat the catalyst under the harsh treatment conditions of 850 ° C. or more and 24 hours or more, it is necessary to provide equipment with safety measures and personnel for monitoring during the treatment. Become. Working with hydrogen at high temperatures is a very dangerous task.
【０００４】本発明の目的は、上記の点に鑑み、触媒製
造コストの増加の要因となる安全対策を施した設備や監
視のための人員の必要がなくかつ活性炭中の官能基を安
全に除去することができるアンモニア合成触媒の製造方
法を提供することにある。SUMMARY OF THE INVENTION In view of the foregoing, it is an object of the present invention to eliminate the need for equipment for safety measures or personnel for monitoring, which causes an increase in catalyst production costs, and to safely remove functional groups in activated carbon. It is an object of the present invention to provide a method for producing an ammonia synthesis catalyst.
【０００５】[0005]
【課題を解決するための手段】本発明によるアンモニア
合成触媒の製造方法は、活性炭に貴金属およびアルカリ
金属、アルカリ土類金属または希土類金属を担持してア
ンモニア合成触媒を得るに当たり、担持前に活性炭をア
ルカリ処理しておくことを特徴とする方法である。The method for producing an ammonia synthesis catalyst according to the present invention is characterized in that activated carbon is supported on a noble metal and an alkali metal, an alkaline earth metal or a rare earth metal to obtain an ammonia synthesis catalyst. This is a method characterized by performing an alkali treatment.
【０００６】担持前の活性炭をアルカリ処理する方法と
しては、予め、約１１０℃で１時間以上乾燥させた活性
炭をＫＯＨ、ＮａＯＨをはじめとするアルカリ金属水酸
化物の水溶液、またはＣａ（ＯＨ）2 、Ｍｇ（ＯＨ）2
等のアルカリ土類金属水酸化物の水溶液に浸漬する方法
が好ましい。浸漬時間は、上記水溶液の濃度、温度等に
もよるが、通常は１〜２４時間である。[0006] As a method of treating the activated carbon before loading with alkali, an activated carbon previously dried at about 110 ° C for 1 hour or more is treated with an aqueous solution of an alkali metal hydroxide such as KOH or NaOH, or Ca (OH) 2. , Mg (OH) 2
The method of immersing in an aqueous solution of an alkaline earth metal hydroxide such as The immersion time is usually 1 to 24 hours, depending on the concentration, temperature, etc. of the aqueous solution.
【０００７】その後、活性炭を充分水洗し、約１１０℃
で１時間以上空気下で乾燥させる。After that, the activated carbon is sufficiently washed with water, and is heated to about 110 ° C.
And dry under air for 1 hour or more.
【０００８】活性炭はハニカム形状に成型されたもので
あることが好ましい。[0008] The activated carbon is preferably formed into a honeycomb shape.
【０００９】貴金属としてはルテニウムが好ましい。た
とえば、アルカリ処理活性炭を、Ｒｕ3 （ＣＯ）12をは
じめとするルテニウムのカルボニル化合物または錯体、
塩化物をはじめとするルテニウムの水溶性化合物を用い
てルテニウムを活性炭に担持する。As a noble metal, ruthenium is preferred. For example, an alkali-treated activated carbon is converted to a ruthenium carbonyl compound or complex including Ru 3 (CO) 12 ,
Ruthenium is supported on activated carbon using a water-soluble compound of ruthenium such as chloride.
【００１０】アルカリ金属、アルカリ土類金属および希
土類金属としては、硝酸塩、炭酸塩をはじめとする水溶
性化合物の形態をなすものが好ましく用いられる。As the alkali metal, alkaline earth metal and rare earth metal, those in the form of water-soluble compounds such as nitrates and carbonates are preferably used.
【００１１】ルテニウムを活性炭に担持するには、ルテ
ニウム換算で１〜４０ｇ／ｌの濃度のルテニウム化合物
溶液に活性炭を１〜２４時間浸漬する方法が好ましい。
この浸漬によって、活性炭へのルテニウム化合物の吸着
現象を利用してルテニウムを担持させることができる。
その後、ルテニウム溶液から活性炭を取り出し、充分垂
れ切りを行った後、約１１０℃で１時間以上空気下で乾
燥する。In order to carry ruthenium on activated carbon, it is preferable to immerse the activated carbon in a ruthenium compound solution having a concentration of 1 to 40 g / l in terms of ruthenium for 1 to 24 hours.
By this immersion, ruthenium can be supported using the adsorption phenomenon of the ruthenium compound to the activated carbon.
Thereafter, the activated carbon is taken out of the ruthenium solution, dripped sufficiently, and then dried at about 110 ° C. for 1 hour or more under air.
【００１２】活性炭に担持したルテニウム化合物からア
ニオンを除去するために、ルテニウムを担持した活性炭
を窒素または水素雰囲気下で温度３５０〜５００℃で１
〜３時間熱処理することが好ましい。この時、熱処理温
度までの昇温速度を１．５〜１０℃／ｍｉｎとすること
が好ましい。In order to remove anions from the ruthenium compound supported on the activated carbon, the activated carbon supported on the ruthenium is heated at 350 to 500 ° C. under a nitrogen or hydrogen atmosphere at a temperature of 350 to 500 ° C.
The heat treatment is preferably performed for up to 3 hours. At this time, it is preferable that the rate of temperature rise up to the heat treatment temperature is 1.5 to 10 ° C./min.
【００１３】次いで、ルテニウム担持活性炭をアルカリ
金属、アルカリ土類金属および希土類金属の硝酸塩、炭
酸塩をはじめとする水溶性化合物の水溶液に１時間以上
浸漬し、アルカリ金属、アルカリ土類金属および希土類
金属をルテニウム担持活性炭に吸着担持する。その後、
これを水溶液から取り出し充分垂れ切りを行った後、約
１１０℃で１時間以上空気下で乾燥する。Next, the activated carbon carrying ruthenium is immersed in an aqueous solution of a water-soluble compound such as a nitrate or a carbonate of an alkali metal, an alkaline earth metal or a rare earth metal for at least one hour, and the alkali metal, the alkaline earth metal and the rare earth metal are immersed. Is adsorbed and supported on ruthenium-supported activated carbon. afterwards,
This is taken out of the aqueous solution, dripped sufficiently, and dried at about 110 ° C. for 1 hour or more under air.
【００１４】乾燥後、水素またはアンモニア合成ガス
（水素＋窒素）の雰囲気下で約４５０℃まで徐々に昇温
し約４５０℃で２時間以上、好ましくは３〜５時間保持
し、担持したアルカリ金属、アルカリ土類金属および希
土類金属の水溶性化合物からアニオンを除去する。After drying, the temperature is gradually raised to about 450 ° C. in an atmosphere of hydrogen or ammonia synthesis gas (hydrogen + nitrogen), and the temperature is maintained at about 450 ° C. for 2 hours or more, preferably 3 to 5 hours. To remove anions from water soluble compounds of alkaline earth metals and rare earth metals.
【００１５】上記方法で調製した触媒は、８５０℃で４
８時間以上水素処理した活性炭を用いた従来の触媒と比
較して、同等またはそれ以上のアンモニア合成活性を示
す。The catalyst prepared by the above method has a temperature of 4 ° C. at 850 ° C.
As compared with a conventional catalyst using activated carbon that has been hydrotreated for 8 hours or more, it exhibits the same or better ammonia synthesis activity.
【００１６】[0016]
【発明の実施の形態】実施例１ （ｉ）バインダーとして酸化珪素−酸化アルミニウムを
約３０％含有する活性炭ハニカムを１１０℃で１時間乾
燥した。乾燥後の重量は、約０．８ｇであった。この乾
燥活性炭ハニカムを１ＮのＫＯＨ水溶液４０ｍｌに２４
時間浸漬した。次いで、同ハニカムを後ＫＯＨ水溶液か
ら取り出し、イオン交換水で水洗後、１００ｍｌのイオ
ン交換水中に２４時間浸漬した。その後、これを後イオ
ン交換水から取り出し１１０℃で１時間乾燥した。EXAMPLE 1 (i) An activated carbon honeycomb containing about 30% of silicon oxide-aluminum oxide as a binder was dried at 110 ° C. for 1 hour. The weight after drying was about 0.8 g. This dried activated carbon honeycomb is added to 40 ml of 1N KOH aqueous solution for 24 hours.
Soaked for hours. Next, the honeycomb was taken out of the KOH aqueous solution, washed with ion-exchanged water, and immersed in 100 ml of ion-exchanged water for 24 hours. Thereafter, this was taken out of the ion-exchanged water and dried at 110 ° C. for 1 hour.
【００１７】（ii）この処理活性炭をルテニウム換算で
１０ｇ／ｌの塩化ルテニウム水溶液２０ｍｌに２４時間
浸漬した。次いで、これを後水溶液から取り出し充分垂
れ切りを行った後、１１０℃で１時間乾燥した。(Ii) This treated activated carbon was immersed in 20 ml of a 10 g / l ruthenium chloride aqueous solution of ruthenium for 24 hours. Next, this was taken out from the post-aqueous solution, sufficiently dripped off, and dried at 110 ° C. for 1 hour.
【００１８】（iii）乾燥後のルテニウム担持活性炭を
水素雰囲気下、１００℃／ｈの速度で２００℃まで昇温
し２００℃にて１時間保持した後、１０℃／ｍｉｎの速
度で４５０℃まで昇温し４５０℃にて２時間保持し、ル
テニウム担持活性炭中の塩素分を除去した。(Iii) The dried ruthenium-supported activated carbon is heated to 200 ° C. at a rate of 100 ° C./h in a hydrogen atmosphere, kept at 200 ° C. for 1 hour, and then heated to 450 ° C. at a rate of 10 ° C./min. The temperature was raised and maintained at 450 ° C. for 2 hours to remove the chlorine content in the activated carbon supporting ruthenium.
【００１９】（iv）上記処理を行ったルテニウム担持活
性炭を０．０９２モル／ｌに調整した硝酸バリウム水溶
液に浸漬した。これをそのまま一晩放置した後、液から
取り出し充分垂れ切りを行った後１１０℃で１時間乾燥
した。(Iv) The treated ruthenium-supported activated carbon was immersed in an aqueous barium nitrate solution adjusted to 0.092 mol / l. This was left as it was overnight, taken out of the liquid, dripped sufficiently, and dried at 110 ° C. for 1 hour.
【００２０】（ｖ）乾燥品をアンモニア合成ガス雰囲気
（Ｈ2 ／Ｎ2 ＝３）下、１０℃／ｍｉｎの速度で４５０
℃まで昇温し、この温度にて２時間保持し触媒中の硝酸
根を除去した。上記処理品を所定の温度まで冷却し、ア
ンモニア合成触媒を得た。(V) The dried product is heated at a rate of 10 ° C./min under an ammonia synthesis gas atmosphere (H 2 / N 2 = 3) at 450 ° C.
C., and kept at this temperature for 2 hours to remove nitrate groups in the catalyst. The treated product was cooled to a predetermined temperature to obtain an ammonia synthesis catalyst.
【００２１】性能試験 アンモニア合成反応速度を測定した。Performance test The reaction rate of ammonia synthesis was measured.
【００２２】上記触媒を用い次の反応条件でアンモニア
の合成反応速度（触媒単位重量当たりの活性）を測定し
た。測定結果を表１に示す。Using the above catalyst, the synthesis reaction rate of ammonia (activity per unit weight of the catalyst) was measured under the following reaction conditions. Table 1 shows the measurement results.
【００２３】 [0023]
【表１】 実施例２ 塩化ルテニウム水溶液の濃度および浸漬時間を変化させ
た点を除いて、実施例１と同様の操作を行い、ルテニウ
ム担持量の異なる触媒を調製した。[Table 1] Example 2 The same operation as in Example 1 was carried out except that the concentration of the ruthenium chloride aqueous solution and the immersion time were changed, to prepare catalysts having different amounts of ruthenium supported.
【００２４】これらの触媒を用い、実施例１と同様の反
応条件で反応速度を測定した。この結果を図１に示す。Using these catalysts, the reaction rates were measured under the same reaction conditions as in Example 1. The result is shown in FIG.
【００２５】[0025]
【発明の効果】本発明によれば、担持前に活性炭をアル
カリ処理しておくことによって、触媒製造コストの増加
の要因となる安全対策を施した設備や監視のための人員
の必要がない上に、活性炭中の官能基を安全に除去する
ことができる。こうして、工業的に操作し易いアンモニ
ア合成触媒の製造方法を提供することができる。According to the present invention, by treating activated carbon with alkali before loading, there is no need for equipment with safety measures or personnel for monitoring which causes an increase in catalyst production cost. In addition, the functional groups in the activated carbon can be safely removed. Thus, it is possible to provide a method for producing an ammonia synthesis catalyst that is industrially easy to operate.
【図１】ルテニウム（Ｒｕ）担持量と反応速度の関係を
示すグラフである。FIG. 1 is a graph showing the relationship between the amount of ruthenium (Ru) carried and the reaction rate.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G069 AA03 AA08 BA03C BA08A BA08B BB04A BB05C BB08C BC01A BC03C BC08A BC38A BC70A BC70B BD12C CB82 EA18 FB16 FC04 GA01 GA05 ──────────────────────────────────────────────────続 き Continued on front page F term (reference) 4G069 AA03 AA08 BA03C BA08A BA08B BB04A BB05C BB08C BC01A BC03C BC08A BC38A BC70A BC70B BD12C CB82 EA18 FB16 FC04 GA01 GA05
Claims (8)
カリ土類金属または希土類金属とを担持してアンモニア
合成触媒を得るに当たり、担持前に活性炭をアルカリ処
理しておくことを特徴とするアンモニア合成触媒の製造
方法。1. An ammonia synthesis catalyst characterized in that, when a noble metal, an alkali metal, an alkaline earth metal or a rare earth metal is supported on an activated carbon to obtain an ammonia synthesis catalyst, the activated carbon is subjected to an alkali treatment before the catalyst is supported. Manufacturing method.
またはアルカリ土類金属水酸化物の水溶液に浸漬した
後、水洗することにより、活性炭をアルカリ処理する請
求項１記載のアンモニア合成触媒の製造方法。2. The method for producing an ammonia synthesis catalyst according to claim 1, wherein the activated carbon before loading is immersed in an aqueous solution of an alkali metal hydroxide or an alkaline earth metal hydroxide and then washed with water to alkali-treat the activated carbon. Method.
である請求項１または２記載のアンモニア合成触媒の製
造方法。3. The method for producing an ammonia synthesis catalyst according to claim 1, wherein the activated carbon is formed into a honeycomb shape.
のいずれかに記載のアンモニア合成触媒の製造方法。4. The method according to claim 1, wherein the noble metal is ruthenium.
The method for producing an ammonia synthesis catalyst according to any one of the above.
り、ルテニウム換算で１〜４０ｇ／ｌの濃度のルテニウ
ム化合物溶液に活性炭を１〜２４時間浸漬する請求項４
記載のアンモニア合成触媒の製造方法。5. The activated carbon is immersed in a ruthenium compound solution having a concentration of 1 to 40 g / l in terms of ruthenium for supporting the ruthenium on the activated carbon for 1 to 24 hours.
A method for producing the ammonia synthesis catalyst as described above.
は水素雰囲気下で温度３５０〜５００℃で１〜３時間熱
処理する請求項５記載のアンモニア合成触媒の製造方
法。6. The method for producing an ammonia synthesis catalyst according to claim 5, wherein the activated carbon supporting ruthenium is heat-treated at a temperature of 350 to 500 ° C. for 1 to 3 hours in a nitrogen or hydrogen atmosphere.
０℃／ｍｉｎとする請求項６記載のアンモニア合成触媒
の製造方法。7. A heating rate up to a heat treatment temperature of 1.5 to 1
The method for producing an ammonia synthesis catalyst according to claim 6, wherein the temperature is 0 ° C / min.
法によって得られたアンモニア合成触媒。8. An ammonia synthesis catalyst obtained by the production method according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35721798A JP3760257B2 (en) | 1998-12-16 | 1998-12-16 | Method for producing ammonia synthesis catalyst and catalyst obtained by the method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35721798A JP3760257B2 (en) | 1998-12-16 | 1998-12-16 | Method for producing ammonia synthesis catalyst and catalyst obtained by the method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000176284A true JP2000176284A (en) | 2000-06-27 |
| JP3760257B2 JP3760257B2 (en) | 2006-03-29 |
Family
ID=18452985
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35721798A Expired - Fee Related JP3760257B2 (en) | 1998-12-16 | 1998-12-16 | Method for producing ammonia synthesis catalyst and catalyst obtained by the method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3760257B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003088759A (en) * | 2001-09-18 | 2003-03-25 | Mitsubishi Paper Mills Ltd | Low temperature oxidation catalyst filter |
| JP2006231229A (en) * | 2005-02-25 | 2006-09-07 | Honda Motor Co Ltd | Ammonia synthesis catalyst and its production method |
| JP2009248009A (en) * | 2008-04-08 | 2009-10-29 | Hitachi Zosen Corp | Method for producing noble metal-supported catalyst |
| CN104084197A (en) * | 2014-07-15 | 2014-10-08 | 福州大学化肥催化剂国家工程研究中心 | Ruthenium system ammonia synthesis catalyst using graphitization activated carbon as carrier and preparation method of catalyst |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2402081A4 (en) | 2009-02-27 | 2012-11-14 | Hitachi Shipbuilding Eng Co | Ammonia decomposition catalyst |
-
1998
- 1998-12-16 JP JP35721798A patent/JP3760257B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003088759A (en) * | 2001-09-18 | 2003-03-25 | Mitsubishi Paper Mills Ltd | Low temperature oxidation catalyst filter |
| JP2006231229A (en) * | 2005-02-25 | 2006-09-07 | Honda Motor Co Ltd | Ammonia synthesis catalyst and its production method |
| JP2009248009A (en) * | 2008-04-08 | 2009-10-29 | Hitachi Zosen Corp | Method for producing noble metal-supported catalyst |
| CN104084197A (en) * | 2014-07-15 | 2014-10-08 | 福州大学化肥催化剂国家工程研究中心 | Ruthenium system ammonia synthesis catalyst using graphitization activated carbon as carrier and preparation method of catalyst |
| CN104084197B (en) * | 2014-07-15 | 2016-04-06 | 福州大学化肥催化剂国家工程研究中心 | A kind of be carrier ruthenium system ammonia synthesis catalyst and the preparation thereof of graphitization active carbon |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3760257B2 (en) | 2006-03-29 |
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