CN101674876B - 在低热质过滤器基底上的scr - Google Patents
在低热质过滤器基底上的scr Download PDFInfo
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- CN101674876B CN101674876B CN2008800137327A CN200880013732A CN101674876B CN 101674876 B CN101674876 B CN 101674876B CN 2008800137327 A CN2008800137327 A CN 2008800137327A CN 200880013732 A CN200880013732 A CN 200880013732A CN 101674876 B CN101674876 B CN 101674876B
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Images
Classifications
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
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- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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Abstract
本发明提供了有效地同时处理颗粒物和NOx的选择性催化还原(SCR)过滤器。还提供了使用SCR过滤器减少柴油机废气中的NOx浓度和颗粒物的方法。该SCR过滤器可以包括包含多根非织造无机纤维的纤维基质壁流过滤器和在该纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂。通过将纤维基质壁流过滤器与菱沸石分子筛SCR催化剂结合,可以在排放物处理系统中使用时在不造成该过滤器上的过度背压的情况下实现高的催化剂载量。
Description
相关申请
本申请要求2007年2月27日提交的名称为“铜CHA沸石催化剂”的美国临时专利申请60/891,835的优先权,其经此引用并入本文。
背景技术
多年来,氮氧化物(NOx)的有害组分已造成大气污染。NOx包含在例如来自内燃机(例如汽车和卡车)、来自燃烧装置(例如用天然气、油或煤供热的发电站)和来自硝酸生产厂的废气中。
已经使用不同方法处理含NOx的气体混合物。一种处理类型涉及氮氧化物的催化还原。可以有两种方法:(1)非选择性还原法,其中使用一氧化碳、氢或低碳烃作为还原剂,和(2)选择性还原法,其中使用氨或氨前体作为还原剂。在选择性还原法中,可以用少量还原剂实现氮氧化物的高度去除。
选择性还原法被称作SCR法(选择性催化还原)。SCR法在大气氧存在下用氨催化还原氮氧化物,主要形成氮气和水蒸气:
4NO+4NH3+O2→4N2+6H2O
2NO2+4NH3+O2→3N2+6H2O
NO+NO2+NH3→2N2+3H2O
柴油机废气含有构成微粒或颗粒物的相材料(液体和固体)以及NOx。通常在柴油机排气系统中提供催化剂组合物和具有该组合物的基底,以将某些或所有这些废气组分转化成无害组分。例如,柴油机排气系统可以含有柴油机氧化催化剂、滤烟器和用于减少NOx的催化剂中的一种或多种。
柴油机废气的颗粒排放物含有三种主要组分。一种组分是固体、干燥的、固体碳质成分或碳烟成分。这种干燥的碳质物引起常与柴油机废气联系在一起的可见碳烟排放。颗粒物的第二组分是可溶有机成分(“SOF”)。可溶有机成分有时被称作挥发性有机成分(“VOF”)。VOF可以根据柴油机废气的温度以蒸气或以气溶胶(液体冷凝物的细滴)形式存在于柴油机废气中。VOF来自两个来源:(1)活塞每次上下时从发动机汽缸壁上扫除的润滑油;和(2)未燃或部分燃烧的柴油燃料。颗粒物的第三组分是硫酸盐成分。硫酸盐成分由柴油燃料中存在的少量硫组分形成。在柴油燃烧过程中形成小比例的SO3,其又迅速与废气中的水结合形成硫酸。硫酸作为与气溶胶形式的微粒的凝相收集或被吸附到其它微粒组分上,由此增加总颗粒物的质量。
发明概要
下面列出本发明的简要概述,以提供对本文所述一些方面的基本理解。此概述不是要求保护的主题的详尽综述。既不是要确定要求保护的主题的关键或重要要素,也不是要描述本发明的范围。其唯一用途是作为后面给出的更详细描述的序言,以简化形式提出要求保护的主题的一些概念。
本文所述的发明涉及有效提供颗粒物和NOx的同时处理的选择性催化还原(SCR)过滤器。本发明还涉及包含该SCR过滤器的排放物处理系统和排放物处理方法。该SCR过滤器可以包括包含多根非织造无机纤维的纤维基质壁流过滤器和在该纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂。通过将纤维基质壁流过滤器与菱沸石分子筛SCR催化剂(其是具有菱沸石结构的SCR催化剂)结合,可以在排放物处理系统中使用时在不造成该过滤器上的过度背压的情况下实现高催化剂载量。
本发明还涉及减少柴油机废气中的NOx浓度和颗粒物的方法。根据要求保护的主题的一个方面,该方法包括将氨或氨前体注入柴油机废气,并使该废气通过SCR过滤器,该SCR过滤器含有纤维基质壁流过滤器和在该纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂,该纤维基质壁流过滤器含有多根非织造无机纤维。
下列描述和附图详细阐述了要求保护的主题的某些示例性方面。但是,这些方面仅指示了本发明的原理的各种使用方式中的几种,且要求保护的主题旨在包括所有这样的方面及其对等物。在联系附图考虑时,从本发明的下列详述中可清楚看出要求保护的主题的其它优点和新颖特征。
附图简述
图1A是根据本说明书的一个方面的纤维基质壁流过滤器的透视图。
图1B是根据本说明书的一个方面的纤维基质壁流过滤器的一部分的剖视图。
图2A和2B是显示根据本说明书的一个方面的用于处理含NOx和颗粒物的废气流的系统的示意图。
图3是根据本说明书的一个方面的减少柴油机废气中的NOx浓度和颗粒物的示例性方法的流程图。
发明详述
本文所述的本发明涉及有效提供颗粒物和NOx的同时处理的选择性催化还原(SCR)过滤器、排放物处理系统、排放物处理方法。使用涂有菱沸石分子筛SCR催化剂的纤维基质壁流过滤器,可以将NOx减少和微粒去除功能整合到单一催化剂制品中。该排放物处理系统使用整合的滤烟器和SCR催化剂,以显著地使该排放物系统所需的重量和体积最小化。此外,由于用在该系统中的催化组合物的选择,可以为各种温度的废气流提供有效的污染物减除。该特征有利于在各种载荷和发动机速度(它们对发动机排出的废气温度具有显著影响)下运行发动机。
本发明可用在需要高过滤效率的用途中。例如,该SCR过滤器适于有效除去排放物处理系统中的颗粒物。本文公开的纤维基质壁流过滤器和菱沸石分子筛SCR催化剂的结合使得壁流基底可负载实用量的SCR催化剂,而不会在排放物处理系统中使用时造成该涂布的过滤器上的过度背压。
与传统的排放物处理技术相比,通过具有低热质的纤维基质壁流过滤器和作为SCR催化剂的疏水性菱沸石分子筛的组合,可以实现排放物处理系统构造的改进的灵活性和较低的与该系统的主动再生相关的燃料成本。通过用该菱沸石分子筛SCR催化剂涂布该过滤器,该过滤器的较低热质可以提供更快的启动(light-off)、对通过SCR反应进行的NOx控制而言在低温下的更好的转化率、和高温稳定性。
该过滤器含有熔结纤维束,以形成壁流深度过滤器。这种结构产生了高的孔隙率,同时实现了良好的过滤效率。即使在该过滤器壁上涂布SCR催化剂后,该涂料也基本不与基底发生负面的相互作用以致不利地影响物理性质。与未涂布的基底相比,这种具有高SCR涂料载量的基质结构仅表现出非常小的背压升高。
经SCR催化剂用氨(NH3)将NOx还原成氮(N2)。通常使用脲形成氨。该过滤器可以提供脲与该催化剂的有效混合。通过改进脲与SCR催化剂在该纤维基质体内的混合,脲的水解进行更快,由此能够更容易地制造的NH3,以与NOx反应。
该纤维基质壁流过滤器可含有多根非织造无机纤维。这些非织造无机纤维可以是任何合适的纤维,只要该纤维在排放物处理过程中可具有耐热性即可。这些非织造无机纤维可具有高熔点、低导热性、低热膨胀系数、耐受热和振动冲击的能力、低密度、高孔隙率和高渗透性中的一个或多个性质。因此,该含有非织造无机纤维的纤维基质壁流过滤器可具有高熔点、低导热性、低热膨胀系数、耐受热和振动冲击的能力、低密度、高孔隙率和高渗透性中的一个或多个性质。
非织造无机纤维的一般实例包括氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维等。氧化铝纤维通常以纤维形式含有大约95重量%或更多且大约97重量%或更少的氧化铝、和大约3重量%或更多且大约5重量%或更少的二氧化硅。氧化铝纤维可通过将前体物质的溶液挤出或纺丝来制造。
二氧化硅纤维通常含有大约90重量%或更多的非晶二氧化硅,并具有低杂质含量。在一个实施方案中,二氧化硅纤维具有低密度(例如大约2.1克/立方厘米或更大和大约2.2克/立方厘米或更小)、高耐熔性(大约1600℃)、低热导率(大约0.1W/m-K)和接近0的热膨胀。
硅铝酸盐纤维通常含有大约40重量%或更多且大约80重量%或更少的氧化铝、大约5重量%或更多且大约25重量%或更少的二氧化硅、和大约0重量%或更多且大约20重量%的铁或镁氧化。
硼硅酸铝纤维通常含有大约40重量%或更多且大约80重量%或更少的氧化铝、大约5重量%或更多且大约25重量%或更少的二氧化硅、和大约1重量%或更多且大约30重量%的三氧化二硼或氧化硼。硼硅酸铝纤维的详情可见于例如美国专利3,795,524,其经此引用并入本文。
该纤维可以具有任何适用于形成该纤维基质壁流过滤器的整料蜂窝结构的平均纤维直径。在一个实施方案中,该纤维具有大约0.5微米或更大和大约50微米或更小的平均纤维直径。在另一实施方案中,该纤维具有大约0.7微米或更大和大约30微米或更小的平均纤维直径。在又一实施方案中,该纤维具有大约1微米或更大和大约20微米或更小的平均纤维直径。
该纤维可以具有任何适用于形成该纤维基质壁流过滤器的整料蜂窝结构的平均拉伸强度。在一个实施方案中,该纤维具有高于大约700MPa(100,000psi)的平均拉伸强度。在另一实施方案中,该纤维具有高于大约1,200MPa(200,000psi)的平均拉伸强度。在又一实施方案中,该纤维具有高于大约1,800MPa(300,000psi)的平均拉伸强度。在再一实施方案中,该纤维具有高于大约2,100MPa(350,000psi)的平均拉伸强度。
该纤维基质壁流过滤器可以以合适的重量百分比含有氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维等。在一个实施方案中,该过滤器的无机纤维部分含有大约50重量%或更多至大约90重量%或更少的二氧化硅纤维、大约5重量%或更多至大约50重量%或更少的氧化铝纤维和大约10重量%或更多至大约25重量%或更少的硼硅酸铝纤维。
在一个实施方案中,该纤维基质壁流过滤器进一步含有添加剂,例如粘合剂和增稠剂。可以添加有机粘合剂和无机粘合剂,例如硼粘合剂,例如氮化硼。或者,可以加入氮化硼以代替硼硅酸铝纤维。例如,该过滤器以与上文所述类似的重量百分比含有二氧化硅纤维、氧化铝纤维和氮化硼。
在一个实施方案中,该过滤器含有由非晶二氧化硅和/或氧化铝纤维以及大约2至大约12重量%氮化硼纤维制成的低密度熔结纤维陶瓷复合材料。低密度熔结陶瓷复合材料的详情可见于例如美国专利5,629,186,其经此引用并入本文。
该纤维基质壁流过滤器的整料蜂窝结构可以通过任何合适的技术形成。在一个实施方案中,通过经由溶胶凝胶技术形成坯件并经由钻孔法在该坯件中形成孔或小室,形成该过滤器。在另一实施方案中,通过挤出技术形成该过滤器。过滤器的制造细节对本发明而言不是关键的。过滤器的制造细节可见于例如美国专利申请公开2004/0079060,其经此引用并入本文。
该纤维基质壁流过滤器可具有相对较低的热质,这又有助于更快的加热和更短的启动(light-off)时间。由于该纤维基质壁流过滤器可迅速加热至催化剂活化温度,因此,该过滤器上的催化剂可迅速开始将废气中的NOx转化成N2。
该纤维基质壁流过滤器可以具有低的在大约200℃至大约800℃之间的热膨胀系数(CTE 200-800)。在一个实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约1×10-6/℃或更高和大约6×10-6/℃或更低的CTE 200-800。在另一实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约2×10-6/℃或更高和大约4.5×10-6/℃或更低的CTE 200-800。在又一实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约3×10-6/℃或更高和大约4×10-6/℃或更低的CTE 200-800。
该纤维基质壁流过滤器也可以具有低的在大约900℃至大约500℃之间的热膨胀系数(CTE 900-500)。在一个实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约200ppm或更高和大约1500ppm或更低的CTE 900-500。在另一实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约300ppm或更高和大约1000ppm或更低的CTE 900-500。在又一实施方案中,含或不合SCR催化剂涂层的该过滤器具有大约350ppm或更高和大约500ppm或更低的CTE 900-500。
该纤维基质壁流过滤器可具有弹性模量或杨氏模量Emod。该壁流过滤器的Emod可以在室温下或在例如200至1000℃的升高的温度下测量。在一个实施方案中,对未涂布的纤维壁流过滤器材料而言,室温Emod值可以为大约0.9至大约1.2Mpsi。在另一实施方案中,该纤维过滤器材料在涂布时可具有大约0.8至大约1.4的室温Emod值。
该纤维基质壁流过滤器可具有断裂强度模量(MOR)。在一个实施方案中,以与ASTM C 1161-02c类似的方式在典型四点弯曲试验中在室温下测量时,含或不含SCR催化剂涂层的该过滤器具有大约1,000psi或更高和大约2,000psi或更低的MOR。在另一实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约1,000psi或更高和大约1,800psi或更低的MOR。在又一实施方案中,含或不含SCR催化剂涂层的该过滤器具有大约1,000psi或更高和大约1,500psi或更低的MOR。
该纤维基质壁流过滤器可具有薄的多孔壁蜂窝结构,流体流经过该蜂窝结构而不会造成背压或该过滤器上的压力的极大升高。该过滤器可具有任何合适的蜂窝小室密度。在一个实施方案中,蜂窝小室密度为大约100个小室/平方英寸或更大和大约400个小室/平方英寸或更小。在另一实施方案中,该过滤器的蜂窝小室密度为大约200个小室/平方英寸或更大和大约300个小室/平方英寸或更小。蜂窝小室形状可以是正方形、三角形、圆形、椭圆形、五边形、七边形、圆环形等。入口通道可大于出口,以降低背压的生成和储灰能力。该蜂窝结构的壁厚可以为大约10密耳或更大和大约40密耳或更小。在另一实施方案中,该蜂窝结构的壁厚可以为大约20密耳或更大和大约30密耳或更小。该蜂窝结构的壁的孔隙率可为大约60%或更大和大约90%或更小。在另一实施方案中,该蜂窝结构的壁的孔隙率为大约70%或更大和大约85%或更小。在又一实施方案中,该蜂窝结构的壁的孔隙率为大约55%或更大和大约70%或更小。孔径可以为大约15微米或更大和大约100微米或更小。在一个实施方案中,孔径可以为大约15微米或更大和大约30微米或更小。
具有上述性质的任何纤维基质壁流过滤器都适用于本发明的实践中。这类纤维基质壁流过滤器的具体实例可见于例如美国专利申请公开2004/0079060、2005/0042151、2006/0120937、2007/0104621、2007/0104622、2007/0104620、2007/0151799、2007/0151233、2007/0107395、2007/0152364、2007/0111878、2007/0141255、2007/0107396、2007/0110645、2007/0108647、2007/0220871、2007/0207070和2007/0104632,它们经此引用并入本文。
分子筛可以是沸石类(沸石)或非沸石类,且沸石类和非沸石类分子筛可具有菱沸石晶体结构,其也被International Zeolite Association称作CHA结构。沸石类菱沸石包括具有近似式(Ca,Na2,K2,Mg)Al2Si4O12·6H2O的天然生成的沸石类网硅酸盐矿物(例如水合硅酸钙铝)。在″ZeoliteMolecular Sieves,″D.W.Breck著,1973由John Wiley & Sons出版(其经此引用并入本文)中描述了沸石类菱沸石的三种合成形式。Breck报道的这三种合成形式是在J.Chem.Soc,第2822页(1956)中,Barrer等人描述的沸石K-G;在英国专利868,846(1961)中描述的沸石D;和在美国专利3,030,181中描述的沸石R,它们经此引用并入本文。
在经此引用并入本文的美国专利4,544,538中描述了通过在传统OH-介质中使用N-烷基-3-喹核醇、N,N,N-三烷基-1-金刚烷基铵阳离子和/或N,N,N-三烷基-外氨基降冰片烷作为引导剂合成沸石类菱沸石的另一合成形式SSZ-13。SSZ-13通常含有大约8至大约50的二氧化硅/氧化铝摩尔比。通过改变合成混合物中反应物的相对比率和/或通过用螯合剂或酸处理该沸石以从沸石晶格中除去铝,可以调节该摩尔比。通过向该合成混合物中加入SSZ-13的晶种,可以加速SSZ-13的结晶和可以减少不合意的污染物的形成。
在经此引用并入本文的美国专利7,264,789中描述了通过使用晶种的胶态悬浮液使菱沸石结构结晶来合成具有菱沸石晶体结构的非沸石类分子筛的合成形式,硅铝磷酸盐34(SAPO-34)。在经此引用并入本文的美国专利6,162,415中描述了制造具有菱沸石结构的另一合成的非沸石类分子筛SAPO-44的方法。具有菱沸石结构的这些沸石类和非沸石类分子筛SSZ-13、SAPO-34和SAPO-44可用作本发明中的SCR催化剂。
菱沸石分子筛可以是疏水的。疏水性菱沸石分子筛是指该菱沸石分子筛本身是疏水的,或该菱沸石分子筛是通过施用合适的疏水润湿剂外涂层而变疏水的亲水菱沸石分子筛(例如,该粒状材料具有亲水芯和疏水外表面)。
通过与疏水润湿剂接触,可以使菱沸石分子筛的表面变疏水。可以使用任何合适的矿物施用法,尤其是在有机体系中,例如在塑料复合材料、薄膜、有机涂料或橡胶中,以使该菱沸石分子筛表面疏水。矿物施用法的细节描述在例如Jesse Edenbaum,Plastics Additives and ModifiersHandbook,Van Nostrand Reinhold,New York,1992,第497-500页中,其关于表面处理材料及其施加的教导经此引用并入本文。
表面处理材料的一般实例包括偶联剂,例如脂肪酸和硅烷。疏水剂的具体实例包括:有机钛酸盐,例如获自Tioxide Chemicals的Tilcom;获自Kenrich Petrochemical,Inc.的有机锆酸盐或铝酸盐偶联剂;有机官能硅烷,例如获自Witco的Silquest产品或获自PCR的Prosil产品;改性有机硅流体,例如获自Shin Etsu的DM-Fluids;和脂肪酸,如获自WitcoCorporation的Hystrene或Industrene产品或获自Henkel Corporation的Emersol产品。在一个实施方案中,使用脂肪酸及其盐(例如硬脂酸和硬脂酸盐)使菱沸石分子筛的粒子表面疏水。
疏水性是指菱沸石分子筛的表面憎水或拒水的物理性质。可以使用接触角测量结果描述疏水性。通过将固着液滴置于光滑表面上时产生的平衡力确定接触角。在三相(固体(S)、液体(L)和蒸气(V))之间的接触点处与凸液滴表面的切线是接触角θ。
固体-蒸气(γSV)、液体-蒸气(γLV)和固体-液体(γSL)的表面张力之间的关系可以通过下列Young′s公式确定:
F=γρcosθ
其中F=润湿力;γ=液体表面张力;且ρ=润湿周长。
如果水微滴在该表面上铺开,则接触角小于90度且该表面亲水。如果该表面疏水,则接触角大于90度。例如,180度是一表面可具有的最大疏水性。
许多表面在与水接触时改变它们的表面能。动态接触角测量提供了前接触角和后接触角。前接触角是与液体初接触时的表面疏水性的测量,而后接触角测量表面已被液体润湿后的疏水性。因此,在一个实施方案中,对本发明而言,用于表示菱沸石分子筛时,“疏水”或“疏水性”是指菱沸石分子筛粒子具有大约90度或更大的前接触角和/或后接触角,在另一实施方案中,菱沸石分子筛粒子具有大约100度或更大的前接触角和/或后接触角。在又一实施方案中,菱沸石分子筛粒子具有大约110度或更大的前接触角和/或后接触角。在再一实施方案中,菱沸石分子筛粒子具有大约120度或更大的前接触角和/或后接触角。
在一个实施方案中,菱沸石分子筛粒子具有大约90度或更大的后接触角。在另一实施方案中,菱沸石分子筛粒子具有大约100度或更大的后接触角,在又一实施方案中,菱沸石分子筛粒子具有大约110度或更大的后接触角。在再一实施方案中,菱沸石分子筛粒子具有大约120度或更大的后接触角。
动态接触角基于Wilhelmy板技术的重力测量原理并通过在动态接触角仪器(其可以测量粉状样品的前接触角和后接触角)上测量来测定。来自ATI Cahn Instruments Inc.的动态接触角分析系统(型号DCA 315)可用于接触角测量。用标准铂校准板测定去离子水的表面张力(γ)。将粉末样品沉积在双面胶带上。用卡尺测定该胶带的周长(ρ)。将该浸渍胶带置于DCA 315中,并在去离子水中以159微米/秒的速率下降和升高两个浸渍周期。可以由第一浸渍周期的前和后润湿滞后曲线测定接触角。
本发明中的菱沸石分子筛可以是离子交换的菱沸石分子筛。该离子交换的菱沸石分子筛的阳离子可以是任何合适的金属阳离子。金属阳离子的实例包括选自由铜、铬、铁、钴、镍、铱、镉、银、金、铂、锰及其混合物组成的组的过渡金属。所得离子交换的菱沸石分子筛可以是Cu交换的菱沸石分子筛、Fe交换的菱沸石分子筛等。
所需离子交换程度不是特别关键的。菱沸石分子筛可以与这类阳离子交换至所交换的阳离子实现所交换的离子与Al阳离子的任何合适比率的程度。在一个实施方案中,离子交换的菱沸石分子筛具有大约0.3的交换的离子/Al原子比或更大。在另一实施方案中,离子交换的菱沸石分子筛具有大约0.6的交换的离子/Al原子比或更大。在又一实施方案中,离子交换的菱沸石分子筛具有大约0.7的交换的离子/Al原子比或更大。在再一实施方案中,离子交换的菱沸石分子筛具有大约0.8的交换的离子/Al原子比或更大。
该离子交换的菱沸石分子筛可以通过使前体菱沸石分子筛的阳离子与其它阳离子交换来形成。可以以任何合适的技术(例如浸渍技术)实现阳离子的交换。可以将前体菱沸石分子筛浸入含有金属物质的可溶盐的溶液中。可以通过添加氢氧化铵调节该溶液的pH值,以诱发金属阳离子沉淀到前体菱沸石分子筛上。例如,将前体菱沸石分子筛在含有可溶盐(例如硝酸铜)的溶液中浸渍足够的时间,以使铜阳离子通过离子交换并入前体菱沸石分子筛中,然后加入氢氧化铵以使该溶液中的铜离子通过沉淀并入前体菱沸石分子筛上。然后可将该菱沸石分子筛洗涤、干燥和煅烧。
在一个实施方案中,本发明中的菱沸石分子筛粒子可以是细碎粒状材料。本文所用的术语“细碎”是指该粒状材料具有大约10微米或更小的中值单粒子粒度。在一个实施方案中,菱沸石分子筛粒子具有下述粒度分布:其中至少大约90重量%具有大约10微米或更小的粒度。在另一实施方案中,菱沸石分子筛粒子具有下述粒度分布:其中至少大约90重量%具有大约3微米或更小的粒度。在又一实施方案中,菱沸石分子筛粒子具有下述粒度分布:至少大约90重量%具有大约1微米或更小的粒度。
可以通过任何合适的技术用菱沸石分子筛涂布该纤维基质壁流过滤器。在一个实施方案中,通过浸渍技术用菱沸石分子筛涂布该纤维基质壁流过滤器。可以将该纤维基质壁流过滤器垂直浸在一部分菱沸石分子筛浆料中。该过滤器顶部可以刚刚高于浆料表面。由此浆料接触各蜂窝壁的入口侧,但防止了其接触各个壁的出口侧。可以使过滤器留在该浆料中大约30秒。将过滤器从浆料中取出,并如下从过滤器中除去过量浆料:首先将其从通道中沥出,然后用压缩空气吹扫(对着浆料渗透方向),然后从浆料渗透方向抽取真空。通过使用这种技术,催化剂浆料渗入过滤器壁,但不会堵塞孔隙以致在最终过滤器中累积过度背压的程度。本文所用的术语“渗入”在用于描述催化剂浆料在过滤器上的分散时,是指催化剂组合物分散在整个过滤器壁中。所得含有菱沸石分子筛SCR催化剂的纤维基质壁流过滤器可以被称作SCR过滤器。
可以将该涂布的过滤器干燥,然后煅烧。在一个实施方案中,该涂布的过滤器在大约100℃干燥并在大约300℃或更高和大约450℃或更低的更高温度下煅烧。在煅烧后,可以通过计算过滤器的涂布和未涂布的重量来确定催化剂载量。可以通过改变涂料浆的固含量来改变催化剂载量。在一个实施方案中,可以进行过滤器在涂料浆中的反复浸渍,然后如上所述除去过量浆料。
该涂布的过滤器可具有任何合适浓度的菱沸石分子筛SCR催化剂组合物,以确保实现所需NOx减少和微粒去除水平和/或确保该催化剂在长期使用中的充足耐用性。在一个实施方案中,SCR催化剂组合物以大约1克/立方英寸或更大和大约3克/立方英寸或更小的浓度沉积在该过滤器上。在另一实施方案中,SCR催化剂组合物以大约1.2克/立方英寸或更大和大约2.8克/立方英寸或更小的浓度沉积在该过滤器上。在又一实施方案中,SCR催化剂组合物以大约1.4克/立方英寸或更大和大约2.6克/立方英寸或更小的浓度沉积在过滤器上。在再一实施方案中,SCR催化剂组合物以大约1.5克/立方英寸或更大和大约2.5克/立方英寸或更小的浓度沉积在过滤器上。
参照附图描述要求保护的主题,其中类似标号在通篇中用于表示类似元件。在下列描述中,为解释说明,阐述许多具体细节以提供对本发明的充分理解。但是,显而易见的是,可以在没有这些具体细节的情况下实施要求保护的主题。在另一些情况下,以方框图形式显示公知结构和装置以便于描述本发明。
图1A和1B显示了纤维基质壁流过滤器100,其具有多个通道102。这些通道102可以被过滤器基底的内壁104管状围住。该过滤器可具有入口端106和出口端108。交替通道可以在入口端106被入口塞110堵塞,在出口端108被出口塞112堵塞,从而在入口106和出口108处形成相反的棋盘图案。气流114通过未堵塞的通道入口116进入,被出口塞112堵住,并经由多孔通道壁104扩散到出口侧118。由于入口塞110,该废气不能在不穿过壁的情况下直接通过该过滤器。
该纤维基质壁流过滤器可以是催化的,因为过滤器的壁上具有或其中含有一种或多种催化材料。催化材料可以仅存在于元件壁的入口侧上、仅存在于出口侧上、存在于入口和出口侧上。该纤维基质壁流过滤器可以在该元件的入口和/或出口壁上含有一层或多层催化材料和一层或多层催化材料的组合。
图2A和2B是显示用于处理含NOx和颗粒物的废气流的系统的示意图。具体而言,图2A显示了使用SCR过滤器处理含NOx和颗粒物的废气流用的示例性排放物处理系统200A。在图2A中,将含气态污染物(包括未燃烃、一氧化碳和NOx)和颗粒物的废气202从发动机204输送到SCR过滤器206。可以在任选在发动机204与SCR过滤器206之间使用氧化催化剂(DOC)208。尽管未显示,系统200A不包括氧化催化剂。在氧化催化剂208中,未燃的气态、非挥发烃(例如挥发性有机成分(VOF))和一氧化碳可以燃烧形成二氧化碳和水。使用该氧化催化剂除去相当大比例的VOF有助于减轻位于该系统中下游的SCR过滤器206上的颗粒物沉积(例如堵塞)。在一个实施方案中,在该氧化催化剂中将废气中的NOx的相当一部分的NO氧化成NO2。
可以经由喷嘴(未显示)将氨和氨前体(例如脲)以喷雾形式注入废气流。在一个实施方案中,显示在一个管道210上的脲的水溶液充当氨前体,其可以与另一管道212上的空气在混合装置(MD)214中混合。阀216可用于计量加入精确量的脲的水溶液,其在废气流中转化成氨。将带有该添加的氨或氨前体的废气流送往SCR过滤器206。在一个实施方案中,在经过SCR过滤器时,NOx组分被SCR过滤器上捕集的颗粒物(例如碳烟饼)转化成NO,然后通过用氨将NO选择性催化还原而将NO转化成氮。
SCR过滤器206也可以大量除去包括碳烟成分和VOF的颗粒物。在一个实施方案中,该SCR过滤器除去大约80重量%或更多的颗粒物。在另一实施方案中,该SCR过滤器除去大约85重量%或更多的颗粒物。在又一实施方案中,该SCR过滤器除去大约90重量%或更多的颗粒物。可以通过过滤器的再生烧除沉积在SCR过滤器206上的颗粒物。
图2B显示了使用SCR过滤器处理含NOx和颗粒物的废气流的另一示例性排放物处理系统200B。在图2B中,排放物处理系统200B包括在SCR过滤器206下游的滑动(slip)氧化催化剂218。该滑动氧化催化剂218可以含有含贱金属和少于大约0.5重量%铂的组合物。该滑动氧化催化剂可用于在任何过量NH3被排放到大气中之前将其氧化。可以任选在发动机与SCR过滤器之间使用氧化催化剂208。
图3显示了减少柴油机废气中的NOx浓度和颗粒物的示例性方法300。在302处,将氨或氨前体注入柴油机废气。在304处,使废气通过SCR过滤器,该SCR过滤器含有纤维基质壁流过滤器和在该纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂,该纤维基质壁流过滤器含有多根非织造无机纤维。在一个实施方案中,该方法进一步包括在将氨或氨前体注入废气之前使该废气通过氧化催化剂。
尽管未显示在图3中,但在一个实施方案中,该纤维基质壁流过滤器含有氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维或其组合中的至少一种。该纤维基质壁流过滤器可具有大约1×10-6/℃或更高和大约6×10-6/℃或更低的热膨胀系数。该纤维基质壁流过滤器可具有大约1,000psi或更高和大约2,000psi或更低的断裂强度模量。在另一实施方案中,该菱沸石分子筛SCR催化剂包含疏水性菱沸石分子筛。该菱沸石分子筛SCR催化剂可含有金属交换的菱沸石分子筛。例如,该菱沸石分子筛SCR催化剂含有Cu交换的菱沸石分子筛、Fe交换的菱沸石分子筛、或其组合中的至少一种。
下列实施例例证本发明。除非在下列实施例中以及在本说明书和权利要求中的其它地方另行指明,所有份数和百分比都按重量计,所有温度都按℃计,且压力等于或接近大气压。
实施例1
实施例1显示了涂布的纤维基质壁流过滤器的背压评测。使用具有1×3英寸的尺寸、15微米平均孔径和67%壁孔隙率的纤维基质壁流过滤器制备催化剂涂布的过滤器。催化剂浆料由铜交换的3%菱沸石分子筛(基于菱沸石分子筛的重量,含有3重量%的铜)和去离子水形成。
如下所述将催化剂沉积在纤维基质壁流过滤器上:(1)将过滤器浸入所述浆料,至足以从一个方向沿该过滤器的整个轴长涂布过滤器通道的深度;(2)从与涂布方向相反的侧(例如干燥侧)对过滤器施以气刀;(3)从涂布侧将该过滤器吸真空;和(4)将该过滤器在流动空气中在大约93℃干燥大约1小时,并将该过滤器在大约400℃煅烧大约1小时。然后从相反侧重复作用(1)至(4)。所得纤维基质壁流过滤器被称作FMWFF。具有三种不同催化剂载量的所得纤维基质壁流过滤器上的压降显示在表1中。
以与对比例类似的方式制备两个堇青石陶瓷壁流过滤器。第一堇青石陶瓷壁流过滤器具有1×6英寸的尺寸、18微米的平均孔径、和59%的壁孔隙率。第二堇青石陶瓷壁流过滤器具有1×6英寸的尺寸、22微米的平均孔径、和65%的壁孔隙率。第一和第二堇青石陶瓷壁流过滤器分别被称作CCWFF1和CCWFF2。堇青石陶瓷壁流过滤器上的压降显示在表1中。
表1
过滤器 | 孔隙率 | 涂布后的压降升高(%) |
FMWFF | 67 | 12至16 |
CCWFF1 | 59 | 36至45 |
CCWFF2 | 65 | 22 |
FMWFF表现出的压降升高低于CCWFF1和CCWFF2的压降。
实施例2
实施例2显示了由涂布的纤维基质壁流过滤器和作为对比例的堇青石陶瓷壁流过滤器(例如SCR过滤器)实现的NOx转化率和NH3转化率的评测。使用实施例1的FMWFF和CCWFF2。两个壁流过滤器部件都具有1×6英寸的尺寸。以实施例1中所述的方式将SCR催化剂以2克/立方英寸的催化剂载量沉积在两个堇青石陶瓷壁流过滤器上。通过将500ppmNO、500ppm NH3、10%O2、5%H2O、余量N2的进料气体混合物添加到含1″Dx3″L催化剂芯的稳态反应器中,由此测量新鲜催化剂芯的氮氧化物选择性催化还原(SCR)效率和选择性。反应在150℃至460℃的温度范围内在40,000hr-1的空速下进行。所得NOx转化率列在表2中。
表2
因此,可以看出,这两个样品之间的催化活性大致等同。
上文已经描述了所公开的信息的实例。当然,为了描述所公开的信息,不可能描述部件或方法的每个可想到的组合,但本领域普通技术人员可以认识到,所公开的信息的许多进一步组合和排列是可行的。相应地,所公开的信息旨在包括落在所附权利要求的实质和范围内的所有这样的改变、修改和变动。此外,在详述或权利要求中使用术语“包括”、“具有”、“涉及”或其变体的情况下,以与“包含”类似的方式,这类术语是非排它的,而“包含”在权利要求中使用时被解释为过渡术语。
Claims (20)
1.选择性催化还原(SCR)过滤器,其包含:
纤维基质壁流过滤器,其含有多根非织造无机纤维;和
在所述纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂。
2.权利要求1的过滤器,其中所述纤维基质壁流过滤器具有蜂窝结构。
3.权利要求1的过滤器,其中所述纤维基质壁流过滤器包含氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维或其组合中的至少一种。
4.权利要求1的过滤器,其中所述纤维基质壁流过滤器具有大约1×10-6/℃或更高和大约6×10-6/℃或更低的从200至800℃的热膨胀系数。
5.权利要求1的过滤器,其中所述纤维基质壁流过滤器具有约50%或更大和大约70%或更小的孔隙率。
6.权利要求1的过滤器,其中所述菱沸石分子筛SCR催化剂包含疏水性菱沸石分子筛。
7.权利要求1的过滤器,其中所述菱沸石分子筛SCR催化剂包含金属交换的菱沸石分子筛。
8.权利要求1的过滤器,其中所述菱沸石分子筛SCR催化剂包含Cu交换的菱沸石分子筛、Fe交换的菱沸石分子筛或其组合。
9.用于处理含NOx和颗粒物的废气流的排放物处理系统,其包含:
将氨或氨前体注入废气流的注射器;和
与所述注射器流体连通并在注射器下游的SCR过滤器,所述SCR过滤器包含纤维基质壁流过滤器和在所述纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂,所述纤维基质壁流过滤器包含多根非织造无机纤维。
10.权利要求9的排放物处理系统,其中所述纤维基质壁流过滤器包含氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维或其组合中的至少一种。
11.权利要求9的排放物处理系统,其中所述纤维基质壁流过滤器具有大约1×10-6/℃或更高和大约6×10-6/℃或更低的从200至800℃的热膨胀系数。
12.权利要求9的排放物处理系统,其中所述纤维基质壁流过滤器具有大约50%或更大和大约70%或更小的孔隙率。
13.权利要求9的排放物处理系统,其中所述菱沸石分子筛SCR催化剂包含疏水性菱沸石分子筛。
14.权利要求9的排放物处理系统,其中所述菱沸石分子筛SCR催化剂包含金属交换的菱沸石分子筛。
15.权利要求9的排放物处理系统,其中所述菱沸石分子筛SCR催化剂包含Cu交换的菱沸石分子筛、Fe交换的菱沸石分子筛或其组合。
16.减少柴油机废气中的NOx和颗粒物的方法,包括:
将氨或氨前体注入柴油机废气;和
使所述废气通过SCR过滤器,该SCR过滤器包含纤维基质壁流过滤器和在所述纤维基质壁流过滤器上的菱沸石分子筛SCR催化剂,所述纤维基质壁流过滤器包含多根非织造无机纤维。
17.权利要求16的方法,进一步包括在将氨或氨前体注入废气之前使所述废气通过氧化催化剂。
18.权利要求16的方法,其中所述纤维基质壁流过滤器包含氧化铝纤维、二氧化硅纤维、莫来石纤维、碳化硅纤维、硅铝酸盐纤维、硼硅酸铝纤维或其组合中的至少一种。
19.权利要求16的方法,其中所述纤维基质壁流过滤器具有大约1×10-6/℃或更高和大约6×10-6/℃或更低的从200至800℃的热膨胀系数。
20.权利要求16的方法,其中所述纤维基质壁流过滤器具有约50%或更大和大约70%或更小的孔隙率。
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JP (3) | JP5592653B2 (zh) |
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