WO2004103554A1 - Jp0407578 catalyseur d'oxydation et d'elimination du methane dans des gaz d'echappement, procede de clarification de gaz d'echappement - Google Patents

Jp0407578 catalyseur d'oxydation et d'elimination du methane dans des gaz d'echappement, procede de clarification de gaz d'echappement Download PDF

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Publication number
WO2004103554A1
WO2004103554A1 PCT/JP2004/007578 JP2004007578W WO2004103554A1 WO 2004103554 A1 WO2004103554 A1 WO 2004103554A1 JP 2004007578 W JP2004007578 W JP 2004007578W WO 2004103554 A1 WO2004103554 A1 WO 2004103554A1
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WIPO (PCT)
Prior art keywords
catalyst
exhaust gas
methane
low
combustion exhaust
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PCT/JP2004/007578
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English (en)
Japanese (ja)
Inventor
Masaki Hondo
Toru Matsui
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Tokyo Gas Co Ltd
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Tokyo Gas Co Ltd
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
    • B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
    • B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/64—Pore diameter
    • B01J35/647—2-50 nm

Definitions

  • the present invention relates to a catalyst for oxidizing and removing methane in a combustion exhaust gas containing a sulfur oxide in a low temperature region, a method for oxidizing and removing methane in a combustion exhaust gas containing a sulfur oxide using the catalyst, and production of the catalyst. About the method.
  • Natural gas, city gas, gas oil, kerosene and other hydrocarbons are used as fuel for boilers, heating furnaces, gas engines and gas turbines. Nitrogen oxides in exhaust gas by burning them fuel (N_ ⁇ _X), sulfur oxides (S_ ⁇ x), carbon monoxide or odor substances, other dust or the like, are contained hydrocarbons' unburned I have. Since these components cause environmental pollution, they must be harmlessly discharged.
  • the treatment method using a three-way catalyst can only be applied effectively to flue gas containing almost no oxygen, and the three-way catalyst has an excess of oxygen and the hydrocarbon in the flue gas is particularly methane. It does not work effectively in some cases.
  • Noble metals such as palladium, platinum, and rhodium are used as hydrocarbon oxidation catalysts. These noble metal catalysts are used in a form supported on a carrier. As carriers are known such as alumina (A l 2 ⁇ 3) Ya Jirukonia (Z r 0 2).
  • Japanese Unexamined Patent Publication No. 2000-330326 and Japanese Unexamined Patent Publication No. 2000-255505 disclose that a catalyst comprising palladium supported on a tin oxide carrier contains sulfur. It has been shown to be highly resistant to inhibition of catalyst activity by oxides.
  • Japanese Patent Application Laid-Open No. 2000-33032 discloses a catalyst comprising palladium and platinum supported on a tin oxide carrier, but platinum is used supplementarily together with palladium. It just does. This point is the same in Japanese Patent Application Laid-Open No. 2001-19093.
  • the temperature of exhaust gas from a lean burn gas engine is lower than 500, usually as low as about 500 to 400 ° C, so that oxidation of methane by an oxidation catalyst is difficult.
  • the oxidation catalyst is significantly deteriorated by poisoning due to the accumulation of a small amount of sulfur oxides contained in exhaust gas. At present, it is not possible to obtain a sufficient durability performance that can be provided for the above. Disclosure of the invention
  • the present inventors have repeatedly experimented and examined various combinations of noble metals such as platinum, ruthenium, and palladium with carriers such as alumina and zirconium and tin oxide carriers.
  • an object of the present invention is to provide a catalyst for removing methane oxidation in a combustion exhaust gas containing sulfur oxide in which platinum is supported on porous tin oxide, and a combustion exhaust gas containing sulfur oxide. Is passed through the oxidation-removal catalyst in a low-temperature range of 500 ° C. or less, particularly in a low-temperature range of 450 ° C. to 350 ° C. to effectively oxidize and remove methane in the combustion exhaust gas for a long period of time. Another object of the present invention is to provide a method for producing the oxidation catalyst.
  • the present invention relates to a catalyst for oxidizing and removing methane in a combustion exhaust gas containing a sulfur oxide in a low temperature range, wherein the oxidation removing catalyst is a catalyst comprising platinum supported on porous tin oxide.
  • the oxidation removing catalyst is a catalyst comprising platinum supported on porous tin oxide.
  • a catalyst for low-temperature oxidation removal of methane in combustion exhaust gas containing sulfur oxides is disclosed.
  • the present invention also relates to a method for oxidizing and removing methane in a combustion exhaust gas containing sulfur oxides in a low temperature range, wherein the combustion exhaust gas is subjected to a low-temperature oxidation removal catalyst comprising platinum supported on porous tin oxide.
  • a low-temperature oxidative removal of methane in combustion exhaust gas containing sulfur oxides characterized in that methane is oxidized and removed by passing through a zone.
  • the present invention relates to a method for producing a catalyst for low-temperature oxidation removal of methane in combustion exhaust gas containing a sulfur oxide obtained by supporting platinum on porous tin oxide, wherein the platinum compound is converted to porous tin oxide.
  • a method for producing a catalyst for low-temperature oxidation and removal of methane in combustion exhaust gas containing sulfur oxides which is supported by an impregnation method or an equilibrium adsorption method with an aqueous solution of a platinum compound and then calcined.
  • the present invention it is possible to support platinum, which does not contain any palladium, which was conventionally considered to be an oxidation-active noble metal of methane, and which is conventionally considered to be ineffective, by itself on porous tin oxide.
  • the oxidation removal catalyst of the present invention has effective durability, the frequency of replacement can be reduced, and the cost of the exhaust gas treatment system can be reduced.
  • FIG. 1 is a diagram showing an example of an apparatus using the oxidation catalyst of the present invention.
  • FIG. 2 is a diagram showing the results of Example 1.
  • FIG. 6 is a diagram showing the results of Example 3.
  • Figure? 8 is a diagram showing the results of Example 4.
  • FIG. 9 is a diagram showing the results of Example 5. BEST MODE FOR CARRYING OUT THE INVENTION
  • the catalyst for oxidizing and removing methane in flue gas according to the present invention is a catalyst in which platinum is supported on porous tin oxide (SnO 2 ). It is a catalyst that is oxidized and removed in a region. According to the present invention, it does not contain any palladium, which has conventionally been regarded as a noble metal active for oxidizing methane, and converts platinum, which was conventionally considered to be ineffective only by itself, into porous tin oxide.
  • methane can be very effectively oxidized and removed over a long period of time in a low temperature range of 500 ° C. or less, particularly in a low temperature range of 450 ° C. to 350 ° C.
  • the method for producing the present oxidation removal catalyst is not particularly limited as long as platinum can be uniformly supported on porous tin oxide, but an impregnation method or an equilibrium adsorption method is preferably applied.
  • the carrier, tin oxide (Sii 2 ) may be any porous material, but it has a peak pore diameter in the range of 20 to 50 nm, and within that range, 60% of the total pore volume. Preferably, it has the above pore volume.
  • a platinum compound is used as a raw material for platinum. Examples include nitrates, chlorides, acetates and complex salts of platinum (tetraammine platinum salt, dinitrodiamine platinum, etc.).
  • a platinum compound is dissolved in water to form an aqueous solution, and a powdery porous tin oxide is added to the aqueous solution and stirred, and the platinum compound is added to the tin oxide.
  • the pH of the aqueous platinum compound solution can be set in a wide range from an acidic region to an alkaline region, but it is preferable to increase the PH value, thereby improving the methane oxidation performance.
  • the pH value is particularly preferably 12 or more. Further, by separately supporting platinum on porous tin oxide, the methane oxidation performance can be remarkably improved.
  • the platinum is divided and supported on the porous tin oxide twice or more with an aqueous solution of a platinum compound. For example, 2 wt% (in terms of platinum) of platinum is loaded at one time, and this loading is repeated several times, such as twice or three times, and loaded at 4 wt% or 6 wt%. It is preferable that the Pt be divided and supported twice or more and five times or less. After that, it is dried and fired by a conventional method.
  • the amount of platinum supported on the tin oxide carrier in the present oxidation catalyst is in the range of 0.025 to 15. Owt%, more preferably 0.8 to 9.0 Owt%, based on tin oxide. It is still effective when the supported amount of platinum is less than 0.025 wt%, but the catalytic effect is reduced accordingly. An effective catalytic effect can also be obtained when the supported amount exceeds about 15.Owt%, but if platinum is supported up to about 15wt%, the desired catalytic effect can be obtained, resulting in cost and other problems. Even from the viewpoint, an upper limit of about 15. Owt% is sufficient. Of course, the above range may be around 0.025 to 15. Owt%. When the oxidation catalyst of the present invention is used in a honeycomb form, an amount corresponding to these is supported.
  • the catalyst should be used in an appropriate form such as powder, granule, granule (including spherical), pellet (cylindrical or annular), tablet (tablet), or honeycomb (monolith). Can be.
  • the powder is sized or granulated in a predetermined particle size range so as not to escape from the catalyst layer filled with the powder.
  • a honeycomb (monolith) form is a preferable form.
  • it is preferably used as a honeycomb.
  • the production mode of the honeycomb catalyst include, for example, (1) supporting a base material having a honeycomb structure by push coating tin oxide thereon, and then supporting an aqueous solution of a platinum compound on the tin oxide-supported honeycomb substrate; ) Tin oxide is dispersed in an aqueous solution of a platinum compound to form a slurry, and the slurry is carried on a honeycomb-shaped substrate by wet coating. Next, it is dried and fired by a conventional method.
  • a ceramic or metal substrate can be used as the substrate in the form of a honeycomb.
  • the ceramic include cordierite
  • the metal include stainless steel and iron-aluminum-chromium alloy.
  • the tin oxide (Sn ⁇ 2 ) carrier according to the present invention has platinum
  • the medium has high S ⁇ x resistance for a long period of time, and contrary to the conventional perception, the presence of SO 2 in the exhaust gas improves the methane oxidation removal activity. The cause is unknown, but it is likely that some significant effect has occurred between tin oxide and platinum or platinum s 2 .
  • FIG. 1 is a diagram showing an example of an apparatus using the oxidation catalyst of the present invention.
  • A is the pipe for introducing the flue gas to be treated
  • B is the oxidation catalyst layer (reaction pipe)
  • C is the pipe for the treated flue gas
  • the arrow (-) indicates the flow direction of the flue gas.
  • the present oxidation catalyst is not limited to the apparatus mode as shown in FIG. 1, but may be used in various apparatus modes as long as it can be disposed for the flue gas flow.
  • the honeycomb-shaped main oxidation catalyst in the catalyst layer as shown in FIG. 1 it is arranged such that its cross-section opening faces the flow direction of the combustion exhaust gas.
  • Example 1 is a diagram showing an example of an apparatus using the oxidation catalyst of the present invention.
  • A is the pipe for introducing the flue gas to be treated
  • B is the oxidation catalyst layer (reaction pipe)
  • C is the pipe for the treated flue gas
  • the arrow (-) indicates the flow direction of the
  • the pellet catalyst was prepared by the impregnation method.
  • the carrier powder is tin oxide raw material (Kanto Chemical Co., Ltd.
  • pellet catalyst carrying and P t to the tin oxide supports, carrying Pd tin oxide pellet catalyst (Pd / S n0 2 pellet catalyst )
  • Pellet catalyst with Pt and Pd supported on alumina Pt-Pd / A
  • the test gas was analyzed using an exhaust gas analyzer (manufactured by Horiba, Ltd.) consisting of a FID total hydrocarbon analyzer, an infrared COZC02 analyzer, a chemiluminescent N ⁇ ⁇ x analyzer, and a magnetic oxygen analyzer.
  • CH 4 oxidation removal activity was evaluated from the difference in CH 4 concentration before and after the reaction tube.
  • Figure 2 shows the results of the performance test at a reaction temperature of 400 ° C.
  • the methane removal rate was 34% in the initial stage, and gradually decreases thereafter, 10% after a lapse of 50 hours, and 2% when 100 hours passed It has dropped to 1% after 140 hours.
  • JP grade shows the 140 hours elapsed until 50 to 53% of the methane removal rate from the initial stage.
  • the Sn_ ⁇ 2 carrier case of Nihon Kagaku Sangyo Co., Ltd. shows a performance analogous thereto.
  • Figure 4 is a graph showing a distribution of pore diameters of the various S N_ ⁇ 2 used in each P t / S n0 2 catalyst described above.
  • Sn_ ⁇ 2 support the most high performance is manufactured by Kanto Chemical Co., Ltd. (special grade), have relatively large pores, its peak represents the 0. 32 c cZg little pore volume in 40 nm.
  • Sn_ ⁇ 2 support this is to follow show the performance Nihon Kagaku Sangyo Co., Ltd. (SL grade), the peak shows a pore volume of 0. 31 cc / g at 3 onm.
  • the peak pore diameter is particularly in the range of 20 to 50 nm. It shows that it is preferable to have a pore volume of 60% or more of the total pore volume.
  • Figure 5 is the P 1; Aru a diagram showing a specific surface area of use Ita various 3110 2 / 311_Rei 2 catalyst. Most shows performance by Kanto Chemical Co. (special grade). For Sn0 2 support, the specific surface area is large, which indicates the value of 13m 2 / g. Also, in the case of Sn_ ⁇ 2 carriers Nihon Kagaku Sangyo Co., Ltd. (SL grades) indicating the performance analogous thereto, shows a value of 12. 5 m 2 _ g.
  • Example 1 Except carrying by dividing the P t is ⁇ Preparation Example Peretsuto catalyst> Example 1, and in the same way to prepare a variety of P t / S N_ ⁇ 2 catalyst.
  • the resulting using each P t / S N_ ⁇ 2 catalyst, in the same manner as the actual Example 1 ⁇ Performance Test>, reaction temperature 400 ° (, was conducted performance tests with SV 160, 00 Oh- 1.
  • Fig. 6 shows the results of this performance test, where Fig.
  • the shown as S n0 2 is the case of the S N_ ⁇ 2 carrier itself carries no P t, which in FIG. 4, to be the same as those shown as Kanto Chemical (special grade).
  • FIG. 8 when carrying the P t at high pH values, shows the pore size distribution close to the pore size distribution of the S n0 2 carrier itself. This is the pH of the Pt compound when loading Pt. Higher values indicate that pore blockage does not occur. In other words, it is shown that the loading of Pt at a high pH value on the Sn— 2 support is effective for improving the main oxidation removal performance.
  • FIG. 9 is a diagram showing the results of this performance test.
  • oxidation removal activity of methane is improved by the presence of S_ ⁇ 2.
  • S_ ⁇ 2 oxidation removal activity of methane is improved by the presence of S_ ⁇ 2.
  • alumina catalyst of the noble metal loaded is known to cause a poisoned performance degradation by S_ ⁇ 2 in the exhaust gas.
  • the oxidation catalyst of the present invention when S_ ⁇ in the exhaust gas 2 is included, let alone performance degradation, oxidation removal activity of methane improves warped.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Catalysts (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

L'invention concerne un catalyseur permettant d'oxyder et d'éliminer le méthane se trouvant dans du gaz de combustion d'échappement contenant des oxydes de soufre dans une gamme de températures basses, lequel comprend de l'oxyde d'étain poreux sur lequel est porté du platine; un procédé d'oxydation et d'élimination du méthane dans du gaz de combustion d'échappement contenant des oxydes de soufre dans une gamme de températures basses de manière efficace sur une longue durée, lequel consiste à utiliser le catalyseur; et un procédé de production du catalyseur. Le catalyseur est complètement exempt de palladium, lequel est un catalyseur à métal noble actif classique pour l'oxydation du méthane, et il contient uniquement du platine, lequel a été considéré par convention comme n'étant pas efficace de lui-même, sous une forme portée par un oxyde d'étain poreux. Le catalyseur peut être utilisé pour oxyder et pour éliminer le méthane de manière extrêmement efficace dans une gamme de basses températures de 500 °C ou moins, notamment, de 450 à 350 °C sur une longue durée, et il peut par conséquent être appliqué à un gaz d'échappement provenant d'un moteur à gaz de combustion dilué utilisant, en tant que carburant, un gaz de ville contenant un composé soufré ainsi qu'un agent conférant une odeur. De plus, le catalyseur présente une durabilité efficace ce qui permet de réduire la fréquence d'échange, conduisant à abaisser le coût d'un système de traitement de gaz d'échappement.
PCT/JP2004/007578 2003-05-26 2004-05-26 Jp0407578 catalyseur d'oxydation et d'elimination du methane dans des gaz d'echappement, procede de clarification de gaz d'echappement Ceased WO2004103554A1 (fr)

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JP2003-148279 2003-05-26
JP2003148279A JP4283037B2 (ja) 2003-05-26 2003-05-26 排ガス中のメタンの酸化除去用触媒及び排ガス浄化方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109562357A (zh) * 2016-08-17 2019-04-02 三井金属矿业株式会社 甲烷氧化催化剂
CN117619378A (zh) * 2023-10-23 2024-03-01 中国科学院大连化学物理研究所 一种耐硫燃烧催化剂及其制备方法和应用

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5541873B2 (ja) * 2008-03-27 2014-07-09 大阪瓦斯株式会社 排ガス浄化用触媒および排ガス浄化方法
EP3673992B1 (fr) 2017-08-22 2024-02-07 Mitsui Mining & Smelting Co., Ltd. Catalyseur d'oxydation du méthane
JP6883135B1 (ja) 2020-05-15 2021-06-09 田中貴金属工業株式会社 メタン燃焼触媒及びその製造方法、並びに燃焼排ガスの浄化方法
JP7038269B1 (ja) 2021-01-07 2022-03-17 田中貴金属工業株式会社 メタン燃焼触媒及びその製造方法、並びに燃焼排ガスの浄化方法
WO2022149319A1 (fr) 2021-01-07 2022-07-14 田中貴金属工業株式会社 Catalyseur de combustion de méthane, son procédé de production, et procédé de nettoyage de gaz d'échappement de combustion

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05146642A (ja) * 1991-12-02 1993-06-15 Osaka Gas Co Ltd 酸化窒素の処理方法及び処理装置
JP2000033266A (ja) * 1998-07-16 2000-02-02 Osaka Gas Co Ltd 炭化水素含有排ガスの浄化用触媒および炭化水素含有排ガスの浄化方法
JP2001190931A (ja) * 2000-01-11 2001-07-17 Osaka Gas Co Ltd メタン含有排ガスの浄化方法
JP2001286764A (ja) * 2000-04-05 2001-10-16 Mitsui Mining & Smelting Co Ltd 排ガス浄化用触媒及びその製造方法
JP2002253969A (ja) * 2001-03-02 2002-09-10 Osaka Gas Co Ltd 排ガス浄化用触媒および排ガス浄化方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05146642A (ja) * 1991-12-02 1993-06-15 Osaka Gas Co Ltd 酸化窒素の処理方法及び処理装置
JP2000033266A (ja) * 1998-07-16 2000-02-02 Osaka Gas Co Ltd 炭化水素含有排ガスの浄化用触媒および炭化水素含有排ガスの浄化方法
JP2001190931A (ja) * 2000-01-11 2001-07-17 Osaka Gas Co Ltd メタン含有排ガスの浄化方法
JP2001286764A (ja) * 2000-04-05 2001-10-16 Mitsui Mining & Smelting Co Ltd 排ガス浄化用触媒及びその製造方法
JP2002253969A (ja) * 2001-03-02 2002-09-10 Osaka Gas Co Ltd 排ガス浄化用触媒および排ガス浄化方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109562357A (zh) * 2016-08-17 2019-04-02 三井金属矿业株式会社 甲烷氧化催化剂
EP3501639A4 (fr) * 2016-08-17 2020-04-01 Mitsui Mining & Smelting Co., Ltd. Catalyseur d'oxydation du méthane
CN109562357B (zh) * 2016-08-17 2022-03-11 三井金属矿业株式会社 甲烷氧化催化剂
CN117619378A (zh) * 2023-10-23 2024-03-01 中国科学院大连化学物理研究所 一种耐硫燃烧催化剂及其制备方法和应用

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