CN102802794A - 多区段催化剂复合物 - Google Patents
多区段催化剂复合物 Download PDFInfo
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- CN102802794A CN102802794A CN2010800267417A CN201080026741A CN102802794A CN 102802794 A CN102802794 A CN 102802794A CN 2010800267417 A CN2010800267417 A CN 2010800267417A CN 201080026741 A CN201080026741 A CN 201080026741A CN 102802794 A CN102802794 A CN 102802794A
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Images
Classifications
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
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Abstract
本发明提供废气处理基材以及包括其的系统和方法。催化剂基材具有流动性能，其中在构造外部外周区段中，相比于外部外周区段，更多的废气流过中间区段。外部外周区段可以在其通道的表面上具有捕获或吸附材料，或者其可以具有相比于内部区段更长的轴长，或者其通道可以具有相比于内部区段更小的开孔。在一个实施方案中，含有捕获材料例如烃阱的外涂层应用于入口端。在另一实施方案中，具有储氧组分的催化剂应用于出口端。
Description
技术领域
本发明总体上涉及具有流动性能的催化剂基材，其中在构造外部外周区段中，相比于外部外周区段，更多的废气流过中间区段。这些基材提供催化功能以及捕获和/或吸附性能。本发明还涉及引入这种催化剂基材的废气处理系统。
背景技术
催化转化器熟知用于除去和/或转化废气的有害组分。对于汽油机，它们典型地含有三元转化(TWC)催化剂，并且位于内燃机的废气线路中。这些催化剂通过氧气促进未燃烧的烃和一氧化碳的废气流中的氧化，以及促进氮氧化物还原为氮气。对于在稀操作条件(lean operating condition)下运行的柴油机，通常提供柴油机氧化催化剂(DOC)，其促进未燃烧的烃和一氧化碳的氧化。
为了该目的，催化转化器具有多种结构。在一种形式中，转化器包括其上具有催化涂层的刚性骨架整体基材。整体具有蜂窝型结构，其具有多个纵向通道(典型为平行的)以提供具有高表面积的催化性涂覆的主体。
含有不同催化剂复合物的整体蜂窝体沿着蜂窝体长度设置在区段中，其用于催化燃烧方法中。层化催化剂结构可通过多种方法制成陶瓷和金属整体式结构。美国专利No.7,189,376(Kumar)中提供多区段催化剂和肼。美国专利No.5,916,133(Buhrmaster)中提供机动车烃吸附剂系统。
在废气线路中，有限的管路空间在例如内燃机和催化转化器之间的肘部，并且导致通过催化转化器的流动的不对称分布。这种流动的不对称分布在瞬时条件的过程中影响催化剂效率和转化。
为了满足不同管理机构设定的更加严格的排放标准，例如提出的SULEV排放规定，有益的是开发催化剂结构，其辅助和促进启动，例如三元转化催化剂的启动。另外，期望完善区段-涂覆技术，并且评价沿着催化剂长度和半径的特定催化剂或污染物吸附剂组合物的置换。
发明概述
本发明的一个或多个方面涉及废气处理催化剂复合物以及包括其的系统和方法。通常，废气处理催化剂复合物包括：
包括第一和第二多个纵向通道的基材，其中所述第一多个通道限定内部径向区带，并且所述第二多个通道限定外部径向区带，
其中所述第一和第二多个纵向通道的内表面包括至少一个催化层，所述催化层包括在负载体上的催化金属，以及
所述第二多个通道被构造为使得相比于所述第二多个通道，更多的废气流过所述第一多个通道。
通过引导更多废气通过外部径向区带，启动可以以这种方式来促进，该方式为不改变催化材料的贵金属分布。在该方式中，废气流动的改变以这种方式实现，该方式为独立于机动车操作系统和催化剂制剂。
在特定实施方案中，在不存在贵金属的条件下所述第二多个通道的内表面还包括含有捕获或吸附材料的层，并且所述第一多个通道的内表面基本上不含所述捕获或吸附材料。
在另一实施方案中，在不存在贵金属的条件下所述第一和第二多个通道的内表面同时还包括含有捕获或吸附材料的层，并且相比于所述第一多个通道，所述第二多个通道具有更长的平均轴长。
附图简述
图1是依照本发明的实施方案的基材示意图；和
图2是依照本发明的实施方案的基材示意图；
图3示意性示出用于涂覆具有径向区带的基材的浸涂盘。
图4A是依照本发明的实施方案的基材示意图；和
图4B是图4A的示意图的剖面。
发明详述
本发明的一个或多个实施方案含有基材，所述基材涂覆含有贵金属的催化材料，例如用于内燃机的催化转化器，其具有径向区段的外周，这被构造以产生不同回压并迫使更多的废气流通过催化转化器的中间区，使得在冷启动过程中，可以促进启动。以以这种方式，更多对流热量集中在中间区以促进更快的加热速度。不同回压可以以多种方式来产生，例如径向区段的外周可以相比于中间区涂覆更多洗涂层材料。另外选择是提供相比于中间区具有更长轴长的外周区。进一步选择是提供相比于中间区在外部区中更小尺寸的通道。通过外周区段的额外洗涂层材料或更长轴长或较小尺寸的开孔产生的限制会控制回压，并且增加流动到催化材料的横截面区域中。这可导致降低通过催化材料的流动的不对称分布(由有限的管路空间例如内燃机和催化转化器之间的肘部引起)。这些结构提供方式来改变不依赖于操作系统和初始含贵金属的催化剂制剂的流动。通过集中通过基材的中间区的流动，外周区域有助于提供绝缘区段以帮助防止热量损失。
当用于描述催化剂基材或区段而涉及″下游″和″上游″时，其是指废气流的流动方向中排气系统中的相对位置。″入口″是指废气进入基材的基材末端，并且″出口″是指废气离开基材的基材末端。
通常，废气处理催化剂复合物包括：包括第一和第二多个纵向通道的基材，其中所述第一多个通道限定内部径向区带，并且所述第二多个通道限定外部径向区带，其中所述第一和第二多个纵向通道的内表面包括至少一个催化层，所述催化层包括在负载体上的催化金属，以及所述第二多个通道被构造为使得相比于所述第二多个通道，更多的废气流过所述第一多个通道。
在特定实施方案中，在不存在贵金属的条件下所述第二多个通道的内表面还包括含有捕获或吸附材料的层，并且所述第一多个通道的内表面基本上不含所述捕获或吸附材料。
在另一实施方案中，在不存在贵金属的条件下所述第一和第二多个通道的内表面同时还包括含有捕获或吸附材料的层，并且相比于所述第一多个通道，所述第二多个通道具有更长的平均轴长。在详细实施方案中，所述第二多个通道的平均长度比所述第一多个通道的平均长度长1cm或所述基材的长度的20％中的较小者。
在一个实施方案中，催化材料包含适于处理内燃机的气态排气流的一种或多种贵金属。例如，可期望提供适于三元转化(TWC)或柴油机氧化的催化材料。催化材料可以由特定内燃机应用所需要的任何组合物和层化结构来构成。
在一个实施方案中，外部径向区带占所述基材的横截面积的约50％、或36％、或甚至20％。
不含贵金属的合适的捕获或吸附材料包括但不限于烃阱、毒物肼、储氧组分。取决于应用，含有捕获或吸附材料的层可以位于催化层之上或之下。例如，烃捕获层可以设置在催化层下。此外，在详细实施方案中，包含所述烃吸附剂的层从所述基材的入口端开始，并且轴向延伸不小于1cm或所述基材的长度的20％中的较小者。在详细实施方案中，提供烃阱层，包括分子筛，例如疏水性沸石。如本文使用的，分子筛例如沸石是指这样的材料，该材料具有基本上均匀的孔分布，其中平均孔尺寸不大于20
。
沸石可以是天然或合成沸石，例如八面沸石、菱沸石、斜发沸石、发光沸石、硅质岩、沸石X、沸石Y、超稳定沸石Y、ZSM-5沸石、ZSM-12沸石、SSZ-3沸石、SAPO5沸石、菱钾铝矿或β沸石。优选的沸石吸附剂材料具有较高氧化硅与氧化铝比例。沸石可具有的氧化硅/氧化铝摩尔比为至少约25/1，优选至少约50/1，有用范围为约25/1至1000/1、50/1至500/1以及约25/1至300/1、约100/1至250/1，或者还例举可选择的约35/1至180/1。优选的沸石包括ZSM、Y和β沸石。特别优选的吸附剂可包括US6,171,556中公开的类型的β沸石。沸石负载量不应该小于0.1g/in3以确保足够的HC储存容量，并且防止在温度跃升之后低温储存过程中储存的石蜡的过早释放。优选地，沸石含量为约0.4至约2.0g/in3，或甚至0.7至1.0g/in3。
在进一步实施方案中，径向区带包括外涂层，其包括毒物肼或吸附剂。毒物肼和吸附剂催化剂是本领域已知的。例如，合适的毒物肼外涂层描述于美国专利申请公开No.2007/0014705，其全部通过引用的方式并入。毒物肼外涂层含有这样的组分，该组分和含有S-、P-、Mn-、C-和/或Fe-的物质相互作用，并且保持这些毒物或重沉积物远离含贵金属的层。这些组分的例子包括掺杂钡、钙、锶、镁和/或铈氧化物的多种氧化铝。其他外涂层材料包括NOx和/或SOx肼，例如一种或多种碱土金属组分。
另外实施方案包括包含储氧组分的外部径向区带。OSC的这种位置提供更多润湿功能效应，并且相对于氧气传感器增加延迟时间，这可是期望的设计特征。这保持烃转化通过含有贵金属的内部径向区带。典型地，储氧组分将包含一种或多种稀土金属的一种或多种可还原氧化物。合适的储氧组分的例子包括氧化铈、氧化镨或其组合。氧化铈递送到层中可以通过使用下列物质来实现，例如氧化铈、铈和锆的混合氧化物、和/或铈、锆和钕的混合氧化物。
在实施方案中，包含储氧组分的层从所述基材的出口端开始，并且轴向延伸不小于1cm或所述基材的长度的20％中的较小者。
在另一方面，提供用于处理包括烃、一氧化碳和其他废气组分的内燃机排气流的排气系统，包括：通过排气集管和所述内燃机流体连接的排气管道；以及根据本发明实施方案的催化剂复合物。
本发明的另一方面包括一种用于处理废气的方法，包括使包含烃、一氧化碳和氮氧化物的气流接触根据本发明实施方案的催化剂复合物。而且，含有源自使用乙醇的氧合物的排气流也可这样处理。
下面提供根据本发明的实施方案的气体处理制品和系统的组件的细节。
现在参照图1，提供具有入口端12和出口端14的基材10。在图1中入口端12具有内部径向区带2和外部径向区带4。至少一个催化层设置在纵向延伸的通道的内表面上，该通道包括内部径向区带2和外部径向区带4。在一个实施方案中，捕获或吸附层设置在外部径向区带4的通道的内表面上，并且沿着基材10的轴长。在图2中，出口端14具有内部径向区带6和外部径向区带8。在另一实施方案中，包含储氧组分的层设置在外部径向区带6的通道的内表面上。
涂覆的基材的一个或多个实施方案可以通过使用改进的浸涂盘来选择性涂覆，该浸涂盘保持涂覆浆料在计量加料涂覆装置中。例如，如图3中所示，浸涂盘可以具有几何形状插入物，其具有附接外环44的固体中间板42，使得当浆料43靠近基材10时，外部径向核心被涂覆，同时内部径向核心保持未涂覆。或者，内部核心的期望尺寸的粘合表面可粘附至基材，以防止进入涂覆浆料。浸涂盘的插入物可被改进以提供任何径向区带涂覆轮廓，例如环。
在图4A和4B中提供具有内部径向区带52和外部径向区带54的基材50，其中外部径向区带54的通道相比于内部径向区带52的通道具有更长的平均轴长。通道长度的差别产生不同回压，从而相比于外部径向区带允许更多流动内部径向区带。两种区段中通道的内表面可以含有层化洗涂层，其中一个层是催化活性的，并且另一个层设置捕获或吸附材料。
载体
在一个或多个实施方案中，一种或多种催化剂复合物设置在载体中。载体可以是那些典型地用于制备催化剂的任何材料，并且将优选包含陶瓷或金属蜂窝结构。可以使用任何合适的载体，例如具有这样类型的整体基材，其具有从基材的入口或出口面延伸通过的微细平行气体流动通道，使得通道对于流过其的流体开放(称为蜂窝流通基材)。从它们流体入口至它们流体出口的基本上直的路径的通道由这样的壁来限定，在该壁上催化材料涂覆为洗涂层，使得流过通道的气体接触催化材料。整体基材的流动通道是薄壁沟道，其可以是任何合适的横截面形状和尺寸，例如梯形、矩形、正方形、正弦、六边形、椭圆形、圆形等。每平方英寸的横截面，这些结构可含有约60至约900或更多的气体入口开孔(即小孔)。
载体还可以是壁流过滤器基材，其中沟道交替地被阻断，从而允许进入沟道的气流从一个方向(入口方向)流过沟道壁，并且从沟道从其他方向(出口方向)离开。双氧化催化剂组合物可涂覆在壁流过滤器上。如果使用这种载体，所得系统将能够除去颗粒物质以及气态污染物。壁流过滤器载体可由本领域通常已知的材料来制备，例如堇青石或碳化硅。
陶瓷载体可以由任何合适的耐火材料制备，例如，堇青石、堇青石-氧化铝、氮化硅、锆石莫来石、锂辉石、氧化铝-氧化硅氧化镁、锆石硅酸盐、矽线石、硅酸镁、锆石、透锂长石、氧化铝、硅铝酸盐等。
用于本发明的催化剂的载体本质上还可以是金属的，并且包括一种或多种金属或金属合金。可以使用多种形状的金属载体，例如皱褶状片或整体形式。优选的金属负载体包括耐热金属和金属合金，例如钛和不锈钢，以及其他合金，其中铁是实质性或主要组分。这些合金可含有镍、铬和/或铝中的一种或多种，并且这些金属的总量可有利地含有至少15重量％的合金，例如10-25重量％的铬、3-8重量％的铝和至多20重量％的镍。所述合金还可含有少量或痕迹量的一种或多种其他金属，例如镁、铜、钒、钛等。金属载体的表面可在高温(例如1000℃或更高)下氧化，以通过在载体表面上形成氧化物层来改善合金的耐腐蚀性。这些高温引起的氧化可增强耐火金属氧化物负载体和催化促进性金属组分与载体的粘附。
在可选择的实施方案中，一种或多种催化剂复合物可沉积在开孔泡沫基材上。这种基材是本领域熟知的，并且典型地由耐火陶瓷或金属材料形成。
层化催化剂复合物的制备
用在基材上的层化催化剂复合物可通过现有技术中熟知的方法容易地制备，例如参见美国专利公开No.2004/0001782，全部通过引用的方式并入本文。下面示出代表性方法。如本文使用的，术语″洗涂层″在本领域的通常意思为施加至基材载体材料的催化或其他材料的薄的粘附性涂层，例如蜂窝型载体构件，其足够多孔以允许待处理的气流通过通道。
催化剂复合物可以容易地制备为整体载体上的层。对于特定洗涂层的第一层，高表面积耐火金属氧化物例如γ氧化铝的细分颗粒在合适的媒介物例如水中制备浆料。然后载体可一次或多种浸渍在这种浆料中，或者浆料可涂覆在载体上，使得沉积在载体上的金属氧化物的期望负载量例如为约0.5至约2.5g/in3。为了引入组分例如贵金属(例如钯、铑、铂和/或其组合)、稳定剂和/或促进剂，这些组分可作为水溶性或水分散性化合物或复合物的混合物引入浆料中。此后，涂覆的载体通过例如在500-600℃下加热约1至约3小时来煅烧。典型地，当期望钯时，钯组分以化合物或复合物的形式来使用，以实现组分分散在耐火金属氧化物负载体例如活化的氧化铝上。为了本发明的目的，术语″钯组分″是指任何化合物、复合物等，其在煅烧或其应用、分解或其他情况时，转化为催化活性形式，通常为金属或金属氧化物。可以使用金属组分的水溶性化合物或水分散性化合物或复合物，只要用于将金属组分浸渍或沉积在耐火金属氧化物负载体颗粒上的液体介质不会不利地和金属或其化合物、或其复合物或其他组分(可存在于催化剂组合物中)反应，并且能够通过在加热和/或施加真空时挥发或分解从金属组分中除去。在一些情况下，直到催化剂使用并且经受在操作过程遇到的高温时，才可发生完全除去液体。通常，从经济和环境方面的观点考虑，使用贵金属的可溶性化合物或复合物的水溶液。例如，合适的化合物是硝酸钯或硝酸铑。在煅烧步骤的过程中，或至少在使用复合物的初始阶段过程中，这些化合物转化为金属或其化合物的催化活性形式。
制备本发明的层化催化剂复合物的任何层的合适方法是制备期望贵金属化合物(例如，钯化合物或钯和铂化合物)和至少一个细分高表面积的耐火金属氧化物负载体例如γ氧化铝的溶液的混合物，其足以干燥以吸附基本上所有溶液以形成湿润固体，该固体稍后联合水以形成可涂覆浆料。在一个或多个实施方案中，浆料是酸性的，pH为约2至小于约7。浆料的pH可通过将足够量的无机或有机酸加入浆料中而降低。当考虑酸和原料的相容性时，可以使用两种的组合。无机酸包括但不限于硝酸。有机酸包括但不限于乙酸、丙酸、草酸、丙二酸、琥珀酸、谷氨酸、己二酸、马来酸、富马酸、邻苯二甲酸、酒石酸、柠檬酸等。此后，如果需要，储氧组分的水溶性或水分散性化合物例如铈-锆复合物、稳定剂例如乙酸钡、和促进剂例如硝酸镧可加入浆料中。
在一个实施方案中，此后浆料粉碎以导致基本上所有固体的粒径为小于约20微米，即平均直径为约0，1-15微米。粉碎可以在球磨机或其他类似设备中完成，并且浆料的固体含量可以为例如约15-60重量％，更具体为约25-40重量％。
附加层可制备，并按照和上述用于将第一层沉积在载体上的相同的方式，沉积在第一层上。
如果需要，催化层还可含有稳定剂和促进剂。合适的稳定剂包括一种或多种不可还原金属氧化物，其中金属选自钡、钙、镁、锶及其混合物。优选地，稳定剂包括钡和/或锶的一种或多种稳定剂。合适的促进剂包括选自镧、镨、钇、锆及其混合物的一种或多种稀土金属的一种或多种不可还原的氧化物。
催化层还可含有储氧组分。典型地，储氧组分将包含一种或多种稀土金属的一种或多种可还原的氧化物。合适的储氧组分的例子包括氧化铈、氧化镨或其组合。氧化铈递送到层中可以通过使用下列物质来实现，例如氧化铈、铈和锆的混合氧化物、和/或铈、锆和钕的混合氧化物。
除非另有说明，在所有情况下，在说明书和权利要求中使用的表达成分、反应条件等的量的所有数值应该理解为由术语″约″所修饰。
径向区段的基材的制备
本发明的径向区段的基材可通过现有技术熟知的方法来容易地制备。代表性方法包括将入口和/或出口端浸渍在洗涂层中，使用模板或模版来将涂料施加至期望的入口径向区域，同时使内部径向区域未涂覆。应该理解，下列方法可根据本发明的不同实施方案来进行改变。
在该说明书中涉及的″一个实施方案″、″某些实施方案″、″一个或多个实施方案″或″实施方案″是指联合实施方案描述的特定特征、结构、材料或特性包括在本发明的至少一个实施方案中。因此，在该说明书中的多个位置出现措词例如″在一个或多个实施方案中″、″在某些实施方案中″、″在一个实施方案中″或″在实施方案中″不必是指本发明的相同实施方案，而且，特定特征、结构、材料或特性可以以任何合适的方式在一个或多个实施方案中联合。
特定涉及上述实施方案和修改形式来描述本发明。在阅读和理解说明书后，可以对其他部分进行进一步的修改和改变。旨在包括所有这些修改和改变，只要它们在本发明的范围内。
Claims (15)
1.一种废气处理催化剂复合物，包含：
包括第一和第二多个纵向通道的基材，其中所述第一多个通道限定内部径向区带，并且所述第二多个通道限定外部径向区带，
其中所述第一和第二多个纵向通道的内表面包括至少一个催化层，所述催化层包括在负载体上的催化金属，以及
所述第二多个通道被构造为使得相比于所述第二多个通道，更多的废气流过所述第一多个通道。
2.权利要求1所述的催化剂复合物，其中在不存在贵金属的条件下所述第二多个通道的内表面还包括含有捕获或吸附材料的层，并且所述第一多个通道的内表面基本上不含所述捕获或吸附材料。
3.权利要求1所述的催化剂复合物，其中在不存在贵金属的条件下所述第一和第二多个通道的内表面还包括含有捕获或吸附材料的层，并且相比于所述第一多个通道，所述第二多个通道具有更长的平均轴长。
4.权利要求1所述的催化剂复合物，其中在不存在贵金属的条件下所述第一和第二多个通道的内表面还包括含有捕获或吸附材料的层，并且相比于所述第一多个通道，所述第二多个通道具有更小的平均开孔周长尺寸。
5.权利要求1所述的催化剂复合物，其中所述外部径向区带至多占所述基材的横截面积的约50％。
6.权利要求2至4中任一项所述的催化剂复合物，其中所述捕获或吸附材料包括烃吸附剂。
7.权利要求6所述的催化剂复合物，其中包含所述烃吸附剂的层位于所述至少一个催化层之下。
8.权利要求6所述的催化剂复合物，其中包含所述烃吸附剂的层从所述基材的入口端开始，并且轴向延伸不小于1cm或所述基材长度的20％中的较小者。
9.权利要求6所述的催化剂复合物，其中所述烃吸附剂包括分子筛，所述分子筛包括选自ZSM-5、Y-沸石、β-沸石及其组合的沸石。
10.权利要求2至4中任一项所述的催化剂复合物，其中所述捕获或吸附材料包含储氧组分，所述储氧组分选自氧化铈、氧化镨及其组合。
11.权利要求10所述的催化剂复合物，其中所述包含储氧组分的层位于所述至少一个催化层之上或之下。
12.权利要求10所述的催化剂复合物，其中所述包含储氧组分的层从所述基材的出口端开始，并且轴向延伸不小于1cm或所述基材的长度的20％中的较小者。
13.权利要求1所述的催化剂复合物，其中所述第二多个通道的平均长度比所述第一多个通道的平均长度长1cm或所述基材的长度的20％中的较小者。
14.一种用于处理包括烃、一氧化碳和其他废气组分的内燃机排气流的系统，该排放物处理系统包括：
通过排气集管和所述内燃机流体连接的排气管道；以及
权利要求1至4中任一项所述的催化剂复合物。
15.一种用于处理废气的方法，包括使包含烃、一氧化碳和氮氧化物的气流接触权利要求1至4中任一项所述的催化剂复合物。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106457146A (zh) * | 2014-04-17 | 2017-02-22 | 巴斯夫公司 | 区域化催化剂复合材料 |
| CN106457146B (zh) * | 2014-04-17 | 2019-12-10 | 巴斯夫公司 | 区域化催化剂复合材料 |
| CN112512687A (zh) * | 2018-11-28 | 2021-03-16 | N.E.化学株式会社 | 废气净化催化剂及其制造方法 |
| CN112512687B (zh) * | 2018-11-28 | 2023-09-22 | N.E.化学株式会社 | 废气净化催化剂及其制造方法 |
| CN116033957A (zh) * | 2020-05-11 | 2023-04-28 | 埃米索尔公司 | 直接捕获基体、装置和方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2419212A2 (en) | 2012-02-22 |
| WO2010121236A3 (en) | 2011-01-13 |
| US8940242B2 (en) | 2015-01-27 |
| CN102802794B (zh) | 2015-01-21 |
| KR20120015321A (ko) | 2012-02-21 |
| US20100263358A1 (en) | 2010-10-21 |
| JP2012523957A (ja) | 2012-10-11 |
| WO2010121236A2 (en) | 2010-10-21 |
| JP2016101581A (ja) | 2016-06-02 |
| EP2419212B1 (en) | 2016-07-06 |
| BRPI1015329A2 (pt) | 2017-10-24 |
| EP2419212A4 (en) | 2014-06-18 |
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