KR100892534B1 - Partial oxidation promoted Diesel Oxidation Catalyst and Method for manufacturing the same - Google Patents
Partial oxidation promoted Diesel Oxidation Catalyst and Method for manufacturing the same Download PDFInfo
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Abstract
본 발명은 디젤 산화촉매에 팔라듐(Pd)과 백금(Pt)을 일정비율 혼합하여 촉매 입구에 코팅함으로써, 디젤연료의 부분 산화를 효율적으로 활성화를 하여 탄화수소, 일산화탄소, 디젤 입자상물질의 제거하는 디젤 산화촉매의 성능을 향상시킴과 더불어 배기가스 온도를 상승시킬 수 있는 디젤 산화촉매 및 그 제조 방법에 관한 것이다.The present invention mixes palladium (Pd) and platinum (Pt) in a diesel oxidation catalyst and coats the catalyst inlet to efficiently activate partial oxidation of diesel fuel to remove hydrocarbons, carbon monoxide and diesel particulate matter. The present invention relates to a diesel oxidation catalyst capable of increasing the performance of the catalyst and increasing the exhaust gas temperature, and to a method of manufacturing the same.
이를 위해, 본 발명은 디젤 산화촉매에서 입구부에서 그 길이방향으로 1/3지점까지 백금과 팔라듐이 1:0~1:3 중량비로 혼합된 귀금속 촉매를 부분 코팅한 것을 특징으로 하는 디젤 산화촉매 및 그 제조 방법을 제공한다To this end, the present invention is a diesel oxidation catalyst characterized in that the diesel oxidation catalyst is partially coated with a noble metal catalyst mixed with platinum and palladium in a weight ratio of 1: 0 to 1: 3 from the inlet to 1/3 of its length in the longitudinal direction. And a method for producing the same.
디젤 산화촉매, 백금, 팔라듐, 질소산화물, 부분산화촉매, 탄화수소. 성상변화 Diesel oxidation catalysts, platinum, palladium, nitrogen oxides, partial oxidation catalysts, hydrocarbons. Change of appearance
Description
본 발명은 상용 디젤자동차를 위한 디젤 산화촉매 및 그 제조방법에 관한 것으로서, 더욱 상세하게는 기존의 하니컴형 코디어라이트 세라믹 담체에 백금(Pt)계 촉매제를 코팅하여 사용하는 일반 디젤 산화촉매보다 성능을 향상시킬 수 있도록 기존의 디젤 산화촉매의 입구부분에 탄화수소를 부분 산화시킬 수 있는 즉, 탄화수소의 가지를 조절하여 배기가스의 성상을 변화시킴과 더불어 산화반응을 향상시키는 개념으로 촉매제를 부분 코팅함으로써, 디젤 산화촉매의 성능 향상과 향후 질소산화물 제거를 위한 조건 형성에 커다란 역할을 할 수 있는 디젤 산화촉매 및 그 제조 방법에 관한 것이다.The present invention relates to a diesel oxidation catalyst for a commercial diesel vehicle and a method of manufacturing the same, and more particularly, to a conventional honeycomb cordierite ceramic carrier, which is coated with a platinum (Pt) -based catalyst and is more effective than a conventional diesel oxidation catalyst. By partially coating the catalyst with the concept of changing the characteristics of the exhaust gas by adjusting the branch of the hydrocarbon and improving the oxidation reaction, it is possible to partially oxidize the hydrocarbon at the inlet of the existing diesel oxidation catalyst to improve the In addition, the present invention relates to a diesel oxidation catalyst which can play a large role in improving performance of diesel oxidation catalyst and forming conditions for removing nitrogen oxide in the future, and a method of manufacturing the same.
특히, 본 발명은 디젤 산화촉매에 팔라듐(Pd)과 백금(Pt)을 일정비율(조건에 따라 조절이 필요함)함께 사용하여 촉매 입구에 코팅함으로써, 상용자동차의 경우 향후 배기가스규제를 만족시키기 위한 시스템에서 고려되는 연료 분사시스템에서 분사되는 디젤연료의 부분 산화를 효율적으로 활성화시켜, 탄화수소, 일산화탄소, 디젤 입자상물질을 용이하게 제거하는 디젤 산화촉매의 성능을 더욱 향상시키고 촉 매 후단의 배기가스 온도를 상승시킬 수 있는 디젤 산화촉매 제조 방법에 관한 것이다.In particular, the present invention by coating the catalyst inlet using a certain ratio (adjustment required depending on the conditions) of palladium (Pd) and platinum (Pt) in the diesel oxidation catalyst, to satisfy future emission regulations in the case of commercial vehicles By effectively activating the partial oxidation of the diesel fuel injected in the fuel injection system considered in the system, the performance of the diesel oxidation catalyst which easily removes hydrocarbons, carbon monoxide and diesel particulate matter can be further improved, and the exhaust gas temperature after the catalyst can be improved. It relates to a method for producing a diesel oxidation catalyst that can be raised.
상용디젤 후처리시스템은 첨부한 도 1에 도시된 바와 같이, 디젤 산화촉매(DOC), 디젤매연여과필터(DPF), 우레아(선택적촉매환원(SCR))시스템으로 구성되어 있으며, 이러한 2차 연료분사를 이용한 상용디젤 후처리시스템에서 상기 디젤 산화촉매는 백금계 촉매제를 세라믹 담체에 균일하게 코팅하는 기술을 이용하여 제조되고 있으며, 그 역할은 배기가스 중 탄화수소, 일산화탄소를 제거하는 것 외에 질소산화물을 산화시킴으로써, 배기온도의 상승에 도움을 주는 역할을 한다.Commercial diesel aftertreatment system is composed of a diesel oxidation catalyst (DOC), diesel particulate filter (DPF), urea (SCR) system, as shown in the accompanying Figure 1, such a secondary fuel In the commercial diesel aftertreatment system using injection, the diesel oxidation catalyst is manufactured using a technology of uniformly coating a platinum-based catalyst on a ceramic carrier, and its role is to remove nitrogen oxides in addition to removing hydrocarbons and carbon monoxide in exhaust gas. By oxidizing, it serves to help raise the exhaust temperature.
종래의 디젤 산화촉매는 향후 적용될 디젤연료를 분사하는 시스템에서 디젤 산화촉매의 산화효율을 증대시키기 위하여 즉, 배기가스 정화효율 증대 및 디젤연료 분사에 의한 배기가스 증가 배출조건을 산화반응에 유리하도록 개선될 필요가 있었다.Conventional diesel oxidation catalyst improves the oxidation efficiency of the diesel oxidation catalyst in the system for injecting diesel fuel to be applied in the future, that is, to improve the exhaust gas purification efficiency and increase the exhaust gas emissions by diesel fuel injection to favor the oxidation reaction Needed to be.
이에, 본 발명자는 디젤연료 분사시스템에서의 디젤 산화촉매의 효율을 증대시키기 위한 연구 노력 결과, 디젤 산화촉매에 백금과 팔라듐의 비율을 조절하고 제오라이트와 알루미나를 적당히 이용하여, 촉매 입구부 즉, 촉매 길이방향 1/3미 만까지 부분 코팅을 하여, 배기가스의 부분 산화촉진, 2차분사에 의해 공급되는 디젤연료를 쉽게 반응할 수 있는 부분 산화촉진을 유도하여, 탄화수소의 성상 및 화학구조를 반응에 유리하게 변경시킴으로써, 산화촉매의 성능 향상과 그에 따른 NO에서 NO2생성 조장으로, 촉매반응에 따른 디젤산화촉매 후단의 배기가스 상승을 유도할 수 있도록 한 디젤 산화촉매 제조 방법을 제공하는데 그 목적이 있다.Accordingly, the present inventors have conducted research to increase the efficiency of diesel oxidation catalysts in diesel fuel injection systems. As a result, by adjusting the ratio of platinum and palladium to diesel oxidation catalysts and using zeolite and alumina as appropriate, Partial coating in less than 1/3 of the longitudinal direction promotes partial oxidation of the exhaust gas and partial oxidation promotion to easily react with diesel fuel supplied by secondary injection, thereby reacting hydrocarbon properties and chemical structure. The present invention provides a method for producing a diesel oxidation catalyst that improves the performance of the oxidation catalyst and thus promotes NO to NO 2 generation, thereby inducing an increase in exhaust gas after the diesel oxidation catalyst due to the catalytic reaction. There is this.
상기한 목적을 달성하기 위한 본 발명의 일 구현예는: 디젤 산화촉매에서 입구부에서 그 길이방향으로 1/3지점까지 백금과 팔라듐이 1:0~1:3 중량비로 혼합된 귀금속 촉매를 부분 코팅한 것을 특징으로 하는 디젤 산화촉매를 제공한다.One embodiment of the present invention for achieving the above object is: Part of a noble metal catalyst in which a platinum and palladium is mixed in a weight ratio of 1: 0 to 1: 3 in a diesel oxidation catalyst from the inlet to 1/3 in the longitudinal direction thereof; It provides a diesel oxidation catalyst characterized in that the coating.
상기한 목적을 달성하기 위한 본 발명의 다른 구현예는: 백금(Pt) 전구체와 팔라듐(Pd) 전구체 용액을 1:0 ~ 1:3 중량비로 혼합하여 알루미나 30g에 함침시킨 후, 열처리하여 백금과 팔라듐을 환원시키는 단계와; 아세트산 27g 및 물 375ml의 혼합용액에 제오라이트 및 상기 환원된 백금과 팔라듐을 침지시킨 다음, 볼밀(Ball mill) 방법으로 입자크기 7 ㎛ 이하인 것이 전체 입자중 94 %가 되도록 밀링하여 고형분이 40 %이고 점도가 300 cpsi인 촉매 슬러리를 얻는 단계와; 상기 촉매 슬러리에 상기 세라믹 모노리스 담체를 길이방향으로 1/3 위치까지 담가서 코팅하는 단계와; 건조로에서 150℃로 2시간 동안 건조하고, 전기로에서 450 ∼ 550℃ 온도로 4시간 동안 소성하는 단계; 를 포함하여 이루어진 것을 특징으로 하는 디젤 산 화촉매 제조 방법을 제공한다.Another embodiment of the present invention for achieving the above object is: a mixture of platinum (Pt) precursor and palladium (Pd) precursor solution 1: 0 ~ 1: 3 by weight ratio, impregnated in 30g of alumina, and then heat treated with platinum Reducing palladium; Zeolite and the reduced platinum and palladium were immersed in a mixed solution of 27 g of acetic acid and 375 ml of water, and then milled to have a particle size of 7 µm or less by 94% of the total particles by a ball mill method, and a solid content of 40% and a viscosity. Obtaining a catalyst slurry having a value of 300 cpsi; Dipping and coating the ceramic monolith carrier in the catalyst slurry to a position in the longitudinal direction to 1/3 position; Drying at 150 ° C. for 2 hours in a drying furnace, and firing at 450 to 550 ° C. for 4 hours in an electric furnace; It provides a diesel oxidation catalyst production method characterized in that it comprises a.
바람직하게는, 상기 제오라이트는 베타제오라이트와 ZSM-5의 비율을 1:1의 중량비로 혼합한 것을 특징으로 한다.Preferably, the zeolite is a mixture of beta zeolite and ZSM-5 in a weight ratio of 1: 1.
상기와 같은 과제 해결 수단을 통하여, 본 발명은 다음과 같은 효과를 제공할 수 있다.Through the problem solving means as described above, the present invention can provide the following effects.
디젤 산화촉매에서 입구부에서 그 길이방향으로 1/3지점까지 백금과 팔라듐이 혼합된 귀금속 촉매를 부분 코팅함으로써, 후처리시스템에서의 디젤 산화촉매의 성능이 보다 향상되고, 내열성이 강화되어, 향후 강화되는 배기규제 대응을 위하여 2차분사계를 이용한 대형차종의 배기 후처리 시스템에 적용될 수 있을 뿐만 아니라 일반 승용 디젤자동차에서도 디젤 산화촉매의 성능향상을 도모할 수 있다.By partially coating the noble metal catalyst mixed with platinum and palladium in the length of the diesel oxidation catalyst from the inlet to one-third of its length, the performance of the diesel oxidation catalyst in the aftertreatment system is further improved and the heat resistance is enhanced. In order to cope with enhanced exhaust regulations, it can be applied to exhaust aftertreatment systems of large vehicles using secondary injection system, and can improve the performance of diesel oxidation catalyst in general passenger diesel vehicles.
또한, 디젤매연필터와 디젤촉매 매연필터를 사용하는 차량에서 이들의 재생조건을 용이하게 만들어 주는 온도 상승에 효과적이며, 선택적 촉매환원반응을 이용한 시스템에서도 운전조건을 효율적으로 하기 위한 온도 조절에 효과적인 장점을 제공할 수 있다.In addition, it is effective to increase the temperature to facilitate their regeneration conditions in vehicles using diesel particulate filter and diesel catalyst soot filter, and effective in controlling temperature for efficient operating conditions even in a system using a selective catalytic reduction reaction. Can be provided.
이하, 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
첨부한 도 2는 본 발명에 따른 디젤 산화촉매의 개념도로서, 본 발명은 기존 디젤 산화촉매의 입구부에서 그 길이방향으로 1/3 지점까지 백금과 팔라듐이 중량비로서 1:0~1:3으로 혼합된 귀금속 촉매를 부분적으로 코팅한 점에 주안점이 있다.2 is a conceptual diagram of a diesel oxidation catalyst according to the present invention, in which the platinum and palladium are 1: 0 to 1: 3 by weight ratio up to one third in the longitudinal direction of the inlet of the existing diesel oxidation catalyst. The focus is on the partial coating of mixed noble metal catalysts.
즉, 본 발명은 백금과 팔라듐을 1:0.1~1:3(예; 1:0.1, 2:1, 3:1, 2:3, 4:1, 5:1, 1:1, 1:2, 1:3 등)의 서로 다른 함량비로 혼합시킨 귀금속 촉매를 제오라이트(베타, ZSM-5등)와 알루미나(감마 알루미나)에 함침시켜 촉매슬러리를 만들고, 이 촉매슬러리를 세라믹 담체에 코팅하여 건조 및 소성을 통해 최종적인 부분 코팅된 디젤 산화촉매를 제공하고자 한 것이다.That is, in the present invention, platinum and palladium are 1: 0.1 to 1: 3 (e.g., 1: 0.1, 2: 1, 3: 1, 2: 3, 4: 1, 5: 1, 1: 1, 1: 2). , 1: 3, etc.) impregnated with a zeolite (beta, ZSM-5, etc.) and alumina (gamma alumina) mixed with a noble metal catalyst mixed in different content ratios to form a catalyst slurry, the catalyst slurry is coated on a ceramic carrier to dry and Firing is to provide a final partially coated diesel oxidation catalyst.
상기 백금과 팔라듐을 포함하는 귀금속의 함량에 대한 비율은 사용되는 조건에서 필요로 하는 탄화수소의 성상변화와 일산화탄소의 부분산화, 즉 공급되는 연료계 또는 후분사에서 발생되는 탄화수소의 종류를 조건에 따라 산화촉매에서 NO2발생에 유리하도록 구성되어야 하므로, 조건에 따라 Pt과 Pd의 비율은 달라질 수 있다.The ratio of the noble metal content containing platinum and palladium is oxidized according to the change in the properties of the hydrocarbon required in the conditions used and the partial oxidation of carbon monoxide, that is, the type of hydrocarbon generated in the fuel system or the post injection supplied. Since the catalyst should be configured to favor the generation of NO 2 , the ratio of Pt and Pd may vary depending on the conditions.
이하, 본 발명을 실시예에 의거하여 더욱 상세하게 설명하겠는바, 본 발명이 하기의 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by the following Examples.
실시예Example
백금 전구체 1g과 팔라듐 전구체 1g이 혼합된 용액을 알루미나 30g에 함침시킨 다음 열처리로에서 환원시켰다.A solution of 1 g of platinum precursor and 1 g of palladium precursor was impregnated into 30 g of alumina and then reduced in a heat treatment furnace.
다음으로, 베타제오라이트와 ZSM-5의 비율을 1:1 중량비로 50g을 혼합하고, 여기에 아세트산 27.0g 및 물 375㎖를 혼합한 용액을 넣었으며, 알루미나에 함침되어 환원된 백금 및 팔라듐을 넣는다.Next, 50 g of beta zeolite and ZSM-5 were mixed in a 1: 1 weight ratio, and a solution containing 27.0 g of acetic acid and 375 ml of water was added thereto, followed by platinum and palladium impregnated with alumina. .
이때 아세트산을 사용하여 pH 4.2로 맞추었다.At this time it was adjusted to pH 4.2 using acetic acid.
상기 제오라이트의 비율은 탄화수소 분해반응 성능에 따른 조합이 가능하므로 특정의 비율 고정에 대한 필요성은 없다.Since the ratio of the zeolite can be combined according to the hydrocarbon decomposition performance, there is no need for a specific ratio fixing.
이어서, 볼밀(Ball mill) 방법으로 입자크기 7㎛ 이하인 것이 전체 입자중 94%가 되도록 밀링하여 고형분이 40 %이고 점도가 300 cpsi인 촉매 슬러리를 얻었으며, 이 범위를 벗어나면 내구성능, 내열성, 초기반응 성능 저하가 발생할 수 있다. Subsequently, a ball mill method was milled to have a particle size of 7 μm or less to 94% of the total particles, thereby obtaining a catalyst slurry having a solid content of 40% and a viscosity of 300 cpsi. If it is out of this range, durability, heat resistance, Deterioration of initial reaction may occur.
여기에, 세라믹 모노리스 담체 즉, 1리터 용량의 400셀의 세라믹 담체에 2 g/ℓ의 백금을 함유한 디젤 산화촉매를 그 입구부부터 길이방향으로 1/3지점까지 상기 촉매 슬러리에 담가서 코팅한 후, 건조로에서 150℃로 2시간 동안 건조하고 전기로에서 450 ∼ 550℃ 온도로 4시간 동안 소성하였다.Here, a ceramic monolith carrier, i.e., a diesel oxidation catalyst containing 2 g / l platinum in a one-liter 400-cell ceramic carrier, was immersed and coated in the catalyst slurry from its inlet to one-third in the longitudinal direction. Then, it was dried for 2 hours at 150 ℃ in a drying furnace and calcined for 4 hours at 450 ~ 550 ℃ temperature in an electric furnace.
비교예Comparative example
기존의 디젤 산화촉매로서, 1리터 용량의 400셀의 세라믹 담체에 2g/ℓ의 백금을 균일하게 코팅한 상업용 디젤산화촉매를 제조하였다.As a conventional diesel oxidation catalyst, a commercial diesel oxidation catalyst was prepared by uniformly coating 2 g / l platinum on a 400-cell ceramic carrier having a capacity of 1 liter.
실험예Experimental Example
실시예 및 비교예에 따른 디젤 산화촉매를 전기로에서 750℃로 에이징(열처리)을 24시간 한 후, 촉매의 활성을 비교하였는 바, 그 결과는 아래의 표 1에 나타낸 바와 같다.After aging (heat treatment) the diesel oxidation catalyst according to Examples and Comparative Examples at 750 ° C. for 24 hours, the activity of the catalysts was compared. The results are shown in Table 1 below.
위에 표 1에서, 저온활성온도는 50% 정화되는 온도로서, 측정된 온도가 낮을 수록 탄화수소, 일산화탄소, 정화효능이 우수함을 의미하며, 활성특성은 각 성분의 제거능력을 나타내는 것으로 높을수록 좋은 특성을 나타낸다.In Table 1 above, the low temperature activity temperature is 50% of the purification temperature, the lower the measured temperature means that the hydrocarbon, carbon monoxide, the purification efficiency is excellent, the higher the activity characteristic indicates the ability to remove each component, the better the characteristics Indicates.
그 결과, 촉매의 활성에서 실시예가 비교예에 비하여 우수한 성능을 나타냄을 알 수 있었다.As a result, it was found that the Example shows better performance than the Comparative Example in the activity of the catalyst.
도 1은 대형 디젤엔진의 후처리 시스템을 설명하는 개념도,1 is a conceptual diagram illustrating the aftertreatment system of a large diesel engine;
도 2는 본 발명에 따른 디젤 산화촉매를 설명하는 개념도.2 is a conceptual diagram illustrating a diesel oxidation catalyst according to the present invention.
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| KR102193496B1 (en) * | 2018-09-21 | 2020-12-21 | (주) 세라컴 | Diesel oxidation catalyst with excellent heat durability and Method thereof |
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| KR20070005406A (en) * | 2005-07-06 | 2007-01-10 | 희성엥겔하드주식회사 | Diesel particulate filter |
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