JP2003251151A - Method for oxidizing/removing fine carbon particle, catalyst and carrier used for the method - Google Patents
Method for oxidizing/removing fine carbon particle, catalyst and carrier used for the methodInfo
- Publication number
- JP2003251151A JP2003251151A JP2002061560A JP2002061560A JP2003251151A JP 2003251151 A JP2003251151 A JP 2003251151A JP 2002061560 A JP2002061560 A JP 2002061560A JP 2002061560 A JP2002061560 A JP 2002061560A JP 2003251151 A JP2003251151 A JP 2003251151A
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- JP
- Japan
- Prior art keywords
- catalyst
- exhaust gas
- tio
- carrier
- fine particles
- 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.)
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Catalysts (AREA)
- Exhaust Gas After Treatment (AREA)
- Processes For Solid Components From Exhaust (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はディーゼルエンジン
排ガス中に含まれるカーボン微粒子の酸化除去方法及び
それに用いる触媒と担体に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for oxidizing and removing carbon fine particles contained in diesel engine exhaust gas, and a catalyst and a carrier used therefor.
【０００２】[0002]
【従来の技術】近年、ディーゼルエンジンからの排ガス
中に含まれるカーボン微粒子による環境汚染の問題が深
刻化している。この問題に対する対策として、フィルタ
ートラップ法や触媒燃焼法等が提案されている。触媒燃
焼法は、エンジンから生じた高温の排ガスを触媒と接触
させて、その排ガス中のカーボン微粒子を酸化燃焼して
CO2に変換させる方法である。このための触媒として、
酸化物系、塩化物系、貴金属系のもの等が提案されてい
る。その中でも白金を触媒とした場合に最も効果的にカ
ーボン微粒子を浄化することが知られている。しかし、
いずれも触媒活性や安定性等の点から未だ満足しうるも
のではなかった。2. Description of the Related Art In recent years, the problem of environmental pollution due to carbon fine particles contained in exhaust gas from diesel engines has become serious. As measures against this problem, a filter trap method, a catalytic combustion method, and the like have been proposed. In the catalytic combustion method, the hot exhaust gas generated from the engine is brought into contact with the catalyst, and the carbon fine particles in the exhaust gas are oxidized and burned.
This is a method of converting to CO 2 . As a catalyst for this,
Oxide type, chloride type, noble metal type, etc. have been proposed. Among them, it is known that when platinum is used as a catalyst, the carbon fine particles are most effectively purified. But,
None of them was still satisfactory in terms of catalytic activity and stability.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、ディーゼル
エンジン排ガス中に含まれるカーボン微粒子を効果的に
酸化除去する方法及びそれに用いる触媒と担体を提供す
ることをその課題とする。An object of the present invention is to provide a method for effectively oxidizing and removing carbon fine particles contained in diesel engine exhaust gas, and a catalyst and a carrier used therefor.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、前記課題
を解決すべく鋭意研究を重ねた結果、本発明を完成する
に至った。即ち、本発明によれば、ディーゼルエンジン
排ガスを触媒と接触させて該排ガス中のカーボン微粒子
を酸化除去する方法において、該触媒として、低温領域
で硫黄酸化物を吸収しNO2とカーボンの反応が活発化す
る300℃付近で硫黄酸化物を放出するものを用いること
を特徴とする前記方法が提供される。該担体として例え
ば、シリカとチタニアの複合酸化物などが提供される。
本発明による触媒と担体がディーゼルエンジン排ガス中
のカーボン微粒子の酸化燃焼に対して高い触媒活性を有
する理由としては、特許第3131630号にあるように、触
媒上で排ガス中に共存するNOが酸化されて生じたNO2が
カーボン微粒子を酸化し、さらにSO2（又はSO3）と水が
この反応を促進することによるものと考えられる。低温
領域でSO3を蓄積しNO2とカーボンの反応が活発化する温
度で放出する担体を用いれば、今後軽油中に含まれる硫
黄分が減少しても高いカーボン酸化性能を望むことがで
きる。The present inventors have completed the present invention as a result of intensive studies to solve the above problems. That is, according to the present invention, in a method of contacting diesel engine exhaust gas with a catalyst to oxidize and remove carbon fine particles in the exhaust gas, as the catalyst, the reaction of NO 2 and carbon by absorbing sulfur oxides in a low temperature region The above-mentioned method is provided, which is characterized by using a material that releases sulfur oxides around 300 ° C which is activated. As the carrier, for example, a composite oxide of silica and titania is provided.
The reason why the catalyst and carrier according to the present invention have high catalytic activity for oxidative combustion of carbon fine particles in diesel engine exhaust gas is that NO existing in exhaust gas is oxidized on the catalyst as described in Japanese Patent No. 3131630. It is considered that NO 2 generated as a result oxidizes the carbon fine particles, and further SO 2 (or SO 3 ) and water promote this reaction. If a carrier that accumulates SO 3 in the low temperature region and releases it at a temperature at which the reaction between NO 2 and carbon is activated is used, it is possible to expect high carbon oxidation performance even if the sulfur content contained in gas oil will decrease in the future.
【０００５】特開平10-211431によれば、SiO2に重量比
で10%以下のTiO2を複合化させた酸化物担体にPtを担持
した触媒がディーゼル排ガス中の炭化水素やSOF分を効
率良く酸化浄化することが報告されている。しかし、こ
の触媒は排ガス中の気相あるいは液相分を対象としたも
のであり、固体カーボン粒子に対する活性については未
だ満足し得るものではない。According to Japanese Unexamined Patent Publication No. 10-211431, a catalyst in which Pt is supported on an oxide carrier in which SiO 2 is mixed with 10% by weight or less of TiO 2 in a weight ratio is effective for hydrocarbons and SOF components in diesel exhaust gas. It has been reported that it is well purified by oxidation. However, this catalyst is intended for the gas phase or liquid phase in the exhaust gas, and its activity with respect to solid carbon particles is not yet satisfactory.
【０００６】[0006]
【発明の実施の形態】本発明の触媒態様は、基材にチタ
ニアおよびシリカを担持し、これに白金を担持させたも
のである。その混合比はTiO2/(TiO2+SiO2)モル比で0.4
〜0.8に調整した場合に最も高い性能を示す。前記担体
金属酸化物としては、対応する金属酸化物の出発物質を
空気中で300〜1000℃、好ましくは500〜700℃で焼成し
たものを用いることができる。この金属酸化物からなる
担体は、粉末状又はペレット状等の各種の形状のもので
あることができる。金属酸化物に対して白金を担持させ
るには、水溶性白金化合物、例えば、Pt(NH3)4(OH)2の
水溶液を金属酸化物に含浸させ、次いで乾燥させた後、
空気中で500〜800℃、好ましくは500〜600℃で焼成す
る。このようにして、担体金属酸化物に白金を担持させ
た触媒を得ることができる。触媒中の白金は、通常、金
属状態で存在し、その含有量は、触媒中、0.05〜20重量
％、好ましくは0.1〜5重量％である。BEST MODE FOR CARRYING OUT THE INVENTION In the catalyst embodiment of the present invention, titania and silica are supported on a substrate, and platinum is supported on the substrate. The mixing ratio is 0.4 in terms of TiO 2 / (TiO 2 + SiO 2 ) molar ratio.
Highest performance when adjusted to ~ 0.8. As the carrier metal oxide, it is possible to use a starting material of the corresponding metal oxide calcined in air at 300 to 1000 ° C, preferably 500 to 700 ° C. The carrier made of this metal oxide can have various shapes such as powder and pellets. In order to support platinum on the metal oxide, a water-soluble platinum compound, for example, Pt (NH 3 ) 4 (OH) 2 is impregnated with an aqueous solution of the metal oxide and then dried,
Baking at 500 to 800 ° C, preferably 500 to 600 ° C in air. In this way, a catalyst in which platinum is supported on a carrier metal oxide can be obtained. Platinum in the catalyst is usually present in a metallic state, and its content is 0.05 to 20% by weight, preferably 0.1 to 5% by weight in the catalyst.
【０００７】本発明の触媒を用いてディーゼルエンジン
排ガス中のカーボン微粒子を酸化除去するためには、そ
の排ガスをその触媒と接触させればよい。この場合の接
触温度は、200〜700℃、好ましくは250〜500℃であり、
接触時間はＧＨＳＶで表わして103〜106hr-1、好ましく
は103〜4×104hr-1である。本発明の触媒と担体は、500
℃以下の比較的低温、特に250〜350℃程度の温度におい
ても高い活性を有し、エンジン排ガスの排出管において
処理するのに好適のものである。In order to oxidize and remove the carbon fine particles in the exhaust gas of a diesel engine using the catalyst of the present invention, the exhaust gas may be brought into contact with the catalyst. The contact temperature in this case is 200 to 700 ° C., preferably 250 to 500 ° C.,
The contact time, expressed in GHSV, is 10 3 to 10 6 hr −1 , preferably 10 3 to 4 × 10 4 hr −1 . The catalyst and carrier of the present invention comprises 500
It has a high activity even at a relatively low temperature of not higher than 0 ° C, particularly at a temperature of about 250 to 350 ° C, and is suitable for treatment in an engine exhaust gas exhaust pipe.
【０００８】実施例
次に本発明を実施例によりさらに詳細に説明する。
（実施例1）粒状炭化珪素（SiC）に金属酸化物担体の出
発物質であるチタニアゾルとシリカゾルモル比でTiO2/
(SiO2＋TiO2)＝0.43になるように含浸し600℃で焼成処
理した後、Pt(NH3)4(OH)2を同様に担持して、触媒と担
体Pt/TiO2-SiO2/SiCを得た（Pt=0.3wt%、TiO2＋SiO2=6w
t%）。模擬排ガス試験は、固定床流通型反応装置を用い
て昇温反応(TPR)を行った。触媒試料0.5gにカーボンブ
ラック(CB)を0.005g混合し、そこへ模擬ディーゼル排ガ
スとして550ppm NO + 15（あるいは1.5ppm）SO2 + 8% H
2O + 10% O2(N2希釈)を1.1L/min流した。80°Cから10°
C/minの速度で昇温し、その間にCBが燃焼することによ
り生成するCO2濃度を非分散型IRで連続分析した。混合
したCBの10%が除去される温度を燃焼開始温度（T10/
℃）と定義し、触媒性能の指標とした。EXAMPLES Next, the present invention will be described in more detail by way of examples. (Example 1) Titan sol, which is a starting material of a metal oxide support, and silica sol were added to granular silicon carbide (SiC) at a molar ratio of TiO 2 /
After impregnation so that (SiO 2 + TiO 2 ) = 0.43 and baking treatment at 600 ° C., Pt (NH 3 ) 4 (OH) 2 was similarly loaded, and the catalyst and carrier Pt / TiO 2 —SiO 2 / SiC was obtained (Pt = 0.3wt%, TiO 2 + SiO 2 = 6w
t%). In the simulated exhaust gas test, a temperature rise reaction (TPR) was performed using a fixed bed flow reactor. 0.005 g of carbon black (CB) was mixed with 0.5 g of catalyst sample, and 550 ppm as simulated diesel exhaust gas there. NO + 15 (or 1.5ppm) SO 2 + 8% H
2 O + Ten% O 2 (diluted with N 2 ) was flowed at 1.1 L / min. 80 ° C to 10 °
The temperature was raised at a rate of C / min, and the CO 2 concentration produced by the combustion of CB during that time was continuously analyzed by a non-dispersive IR. The temperature at which 10% of the mixed CB is removed is the combustion start temperature (T 10 /
℃) and used as an index of catalyst performance.
【０００９】（実施例2）実施例1でTiO2/(SiO2＋TiO2)
＝0.5にした以外は同様に触媒と担体を調製し活性を調
べた。
（実施例3）実施例1でTiO2/(SiO2＋TiO2)＝0.6にした以
外は同様に触媒と担体を調製し活性を調べた。
（実施例4）実施例1でTiO2/(SiO2＋TiO2)＝0.67にした
以外は同様に触媒と担体を調製し活性を調べた。
（実施例5）実施例1でTiO2/(SiO2＋TiO2)＝0.75にした
以外は同様に触媒と担体を調製し活性を調べた。Example 2 In Example 1, TiO 2 / (SiO 2 + TiO 2 )
A catalyst and a carrier were prepared in the same manner except that the ratio was set to 0.5, and the activity was examined. Example 3 A catalyst and a carrier were prepared in the same manner as in Example 1 except that TiO 2 / (SiO 2 + TiO 2 ) = 0.6 was used, and the activity was examined. Example 4 A catalyst and a carrier were prepared in the same manner as in Example 1 except that TiO 2 / (SiO 2 + TiO 2 ) = 0.67 was used, and the activity was investigated. Example 5 A catalyst and a carrier were prepared in the same manner as in Example 1 except that TiO 2 / (SiO 2 + TiO 2 ) = 0.75 was prepared, and the activity was examined.
【００１０】（比較例1）実施例1で担体をSiO2単味にし
た以外は同様に触媒と担体を調製し活性を調べた。
（比較例2）実施例1で担体をTiO2単味にした以外は同様
に触媒と担体を調製し活性を調べた。
（比較例3）実施例1でTiO2/(SiO2＋TiO2)＝0.11にした
以外は同様に触媒と担体を調製し活性を調べた。
（比較例4）実施例1でTiO2/(SiO2＋TiO2)＝0.25にした
以外は同様に触媒と担体を調製し活性を調べた。
（比較例5）実施例1でTiO2/(SiO2＋TiO2)＝0.90にした
以外は同様に触媒と担体を調製し活性を調べた。Comparative Example 1 A catalyst and a carrier were prepared in the same manner as in Example 1 except that the carrier was made of SiO 2 , and the activity was examined. (Comparative Example 2) A catalyst and a carrier were prepared in the same manner as in Example 1 except that the carrier was made of TiO 2 , and the activity was examined. Comparative Example 3 A catalyst and a carrier were prepared in the same manner as in Example 1 except that TiO 2 / (SiO 2 + TiO 2 ) = 0.11 was used, and the activity was examined. (Comparative Example 4) A catalyst and a carrier were prepared in the same manner except that TiO 2 / (SiO 2 + TiO 2 ) = 0.25 was used in Example 1, and the activity was examined. (Comparative Example 5) A catalyst and a carrier were prepared in the same manner as in Example 1 except that TiO 2 / (SiO 2 + TiO 2 ) = 0.90, and the activity was examined.
【００１１】得られた試料の比表面積および白金分散度
およびカーボン燃焼開始温度（T10/℃）の結果を表１に
示す。Table 1 shows the results of the specific surface area, platinum dispersity, and carbon combustion start temperature (T 10 / ° C.) of the obtained sample.
【表１】 [Table 1]
【００１２】実施例４で得られた触媒と担体の硫酸の効
果発現特性を調べるため、TPR反応ガス（SO2＝1.5ppm）
条件下、200℃3hで保持し硫酸を蓄積した後、通常のTPR
を行い同様にカーボン酸化性能を調べた。硫酸蓄積前後
の燃焼開始温度（T10/℃）を比較例１と比較した結果を
表２示す。In order to investigate the effect-producing characteristics of the catalyst and the carrier obtained in Example 4 of sulfuric acid, TPR reaction gas (SO 2 = 1.5 ppm)
Under conditions, hold at 200 ℃ for 3h to accumulate sulfuric acid, and then use normal TPR
Then, the carbon oxidation performance was examined in the same manner. The results of comparison of the combustion start temperature (T 10 / ° C.) before and after the sulfuric acid accumulation with Comparative Example 1 are shown in Table 2.
【表２】
比較例１では硫酸蓄積前後でまったく性能が変化しない
のに対し、実施例４では硫酸蓄積後、50℃以上も低い温
度でカーボン酸化性能を示した。[Table 2] In Comparative Example 1, the performance was not changed before and after the sulfuric acid was accumulated, whereas in Example 4, the carbon oxidation performance was exhibited at a temperature as low as 50 ° C. or higher after the sulfuric acid was accumulated.
【００１３】[0013]
【発明の効果】本発明の触媒と担体の組み合わせによれ
ば、ディーゼルエンジン排ガス中のカーボン微粒子を低
温度で効率よく酸化除去することができる。According to the combination of the catalyst and the carrier of the present invention, it is possible to efficiently oxidize and remove fine carbon particles in the exhaust gas of a diesel engine at a low temperature.
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｆ０１Ｎ 3/10 Ｂ０１Ｄ 53/36 ＺＡＢ (72)発明者 大井 明彦 茨城県つくば市東１−１−１ 独立行政法 人産業技術総合研究所つくばセンター内 (72)発明者 難波 哲哉 茨城県つくば市東１−１−１ 独立行政法 人産業技術総合研究所つくばセンター内 Ｆターム(参考） 3G090 AA03 AA06 3G091 AA18 AB02 AB08 BA13 BA14 GB06W GB10X GB17X 4D048 AA14 AB01 BA06X BA07X BA30X BA42X BA45X CC38 EA04 4G069 AA03 BA02A BA02B BA04A BA04B BA20A BA20B BB02A BB02B BB15A BB15B BC75A BC75B BD05A BD05B CA02 CA03 CA07 CA18 DA06 EC02Y FC08 Continuation of front page (51) Int.Cl. 7 Identification code FI theme code (reference) F01N 3/10 B01D 53/36 ZAB (72) Inventor Akihiko Oi 1-1-1 Higashi, Tsukuba, Ibaraki (72) Inventor Tetsuya Namba, 1-1-1 East, Tsukuba City, Ibaraki Prefecture GB10X GB17X 4D048 AA14 AB01 BA06X BA07X BA30X BA42X BA45X CC38 EA04 4G069 AA03 BA02A BA02B BA04A BA04B BA20A BA20B BB02A BB02B BB15A BB15B BC75A BC75B BD05A BD05B CA02 CA03 CA07 CA18 DA08
Claims (5)
させて該排ガス中のカーボン微粒子を酸化除去する方法
において、白金触媒と、低温領域で硫黄酸化物を吸収し
NO2とカーボンの反応が活発化する300℃付近で硫黄酸化
物を放出する担体を用いることを特徴とする固体カーボ
ン微粒子の酸化除去方法。1. A method for contacting a diesel engine exhaust gas with a catalyst to oxidize and remove carbon fine particles in the exhaust gas, wherein a platinum catalyst and sulfur oxide are absorbed in a low temperature region.
A method for oxidizing and removing solid carbon fine particles, which comprises using a carrier that releases sulfur oxides at around 300 ° C. where the reaction between NO 2 and carbon is activated.
させて該排ガス中のカーボン微粒子を酸化除去する方法
において、白金触媒と、チタニアとシリカを0.4から0.8
の割合（＝TiO2/(TiO2+SiO2)；モル比）で複合した酸化
物の担体を用いることを特徴とする固体カーボン微粒子
の酸化除去方法。2. A method for contacting a diesel engine exhaust gas with a catalyst to oxidize and remove carbon fine particles in the exhaust gas, wherein the platinum catalyst, titania and silica are 0.4 to 0.8.
A method for oxidizing and removing solid carbon fine particles, which comprises using a carrier of an oxide compounded at a ratio of (= TiO 2 / (TiO 2 + SiO 2 ); molar ratio).
させて該排ガス中のカーボン微粒子を酸化除去する方法
において、白金触媒と、炭化珪素にチタニアとシリカを
複合した酸化物の担体を用いることを特徴とする固体カ
ーボン微粒子の酸化除去方法。3. A method of contacting diesel engine exhaust gas with a catalyst to oxidize and remove fine carbon particles in the exhaust gas, wherein a platinum catalyst and an oxide carrier composed of silicon carbide and titania and silica are used. A method for oxidizing and removing solid carbon fine particles.
させて該排ガス中のカーボン微粒子を酸化除去するのに
用いる白金触媒と、チタニアとシリカを0.4から0.8の割
合（＝TiO2/(TiO2+SiO2)；モル比）で複合した酸化物の
担体。4. A platinum catalyst used for contacting diesel engine exhaust gas with a catalyst to oxidize and remove fine carbon particles in the exhaust gas, and titania and silica in a ratio of 0.4 to 0.8 (= TiO 2 / (TiO 2 + SiO 2 ). 2 ); oxide support complexed in molar ratio).
させて該排ガス中のカーボン微粒子を酸化除去するのに
用いる白金触媒と、炭化珪素にチタニアとシリカを複合
した酸化物の担体。5. A platinum catalyst used for contacting diesel engine exhaust gas with a catalyst to oxidize and remove carbon fine particles in the exhaust gas, and an oxide carrier composed of silicon carbide and titania and silica.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002061560A JP3994153B2 (en) | 2002-03-07 | 2002-03-07 | Method for oxidizing and removing solid carbon fine particles, and catalyst and carrier used therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002061560A JP3994153B2 (en) | 2002-03-07 | 2002-03-07 | Method for oxidizing and removing solid carbon fine particles, and catalyst and carrier used therefor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003251151A true JP2003251151A (en) | 2003-09-09 |
| JP3994153B2 JP3994153B2 (en) | 2007-10-17 |
Family
ID=28670371
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|---|---|---|---|
| JP2002061560A Expired - Lifetime JP3994153B2 (en) | 2002-03-07 | 2002-03-07 | Method for oxidizing and removing solid carbon fine particles, and catalyst and carrier used therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013031682A1 (en) * | 2011-08-26 | 2013-03-07 | 住友大阪セメント株式会社 | Exhaust purification catalyst, exhaust gas purifier of internal combustion engine, and exhaust gas purification filter |
| JP2013063421A (en) * | 2011-08-26 | 2013-04-11 | Sumitomo Osaka Cement Co Ltd | Exhaust purification catalyst and exhaust gas purifier of internal combustion engine |
| JP2013515199A (en) * | 2009-12-22 | 2013-05-02 | パーキンズ エンジンズ カンパニー リミテッド | Sulfur detection routine |
-
2002
- 2002-03-07 JP JP2002061560A patent/JP3994153B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013515199A (en) * | 2009-12-22 | 2013-05-02 | パーキンズ エンジンズ カンパニー リミテッド | Sulfur detection routine |
| WO2013031682A1 (en) * | 2011-08-26 | 2013-03-07 | 住友大阪セメント株式会社 | Exhaust purification catalyst, exhaust gas purifier of internal combustion engine, and exhaust gas purification filter |
| JP2013063421A (en) * | 2011-08-26 | 2013-04-11 | Sumitomo Osaka Cement Co Ltd | Exhaust purification catalyst and exhaust gas purifier of internal combustion engine |
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|---|---|
| JP3994153B2 (en) | 2007-10-17 |
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