CN1229307C - 堵塞陶瓷蜂窝体中通道的方法 - Google Patents
堵塞陶瓷蜂窝体中通道的方法 Download PDFInfo
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- CN1229307C CN1229307C CNB028103351A CN02810335A CN1229307C CN 1229307 C CN1229307 C CN 1229307C CN B028103351 A CNB028103351 A CN B028103351A CN 02810335 A CN02810335 A CN 02810335A CN 1229307 C CN1229307 C CN 1229307C
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- mixture
- ceramic honeycomb
- honeycomb body
- ceramic
- passage
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Images
Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
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- B01D53/34—Chemical or biological purification of waste gases
- 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
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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- B01D—SEPARATION
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- B01D53/34—Chemical or biological purification of waste gases
- 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
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/9454—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific device
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/003—Apparatus or processes for treating or working the shaped or preshaped articles the shaping of preshaped articles, e.g. by bending
- B28B11/006—Making hollow articles or partly closed articles
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- C—CHEMISTRY; METALLURGY
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Abstract
由包括如下步骤的方法，通过堵塞陶瓷蜂窝体中的通道而制备陶瓷蜂窝壁流过滤器。首先，形成包括分散液体和陶瓷粉末的混合物。其次，在未堵塞的陶瓷蜂窝体中的通道的一端中***该混合物，使得该混合物流到另一端，在那里混合物聚集和形成堵塞的陶瓷蜂窝体。然后，加热堵塞的陶瓷蜂窝体到足以烧结堵塞的陶瓷蜂窝体的温度，以形成多孔的烧结的堵塞的陶瓷蜂窝体。
Description
本申请要求2001年4月23日提交的U.S.临时申请系列No.60/258,809的权益。
技术领域
本发明涉及陶瓷壁流过滤器及其制造方法。具体而言，本发明涉及颗粒捕集器，如柴油颗粒捕集器。
背景技术
由于空气质量标准更为严格，相当的努力着力于最小化柴油发动机排气中释放的粒状物质。潜在的解决方案是***柴油发动机排气***中的颗粒捕集器。
如在U.S.专利No.4,276,071中描述的蜂窝陶瓷壁流通过滤器，是颗粒捕集器的优选类型。这些蜂窝过滤器由如下方式制造：挤出由水，粘合剂和陶瓷粉末(例如粘土、莫来石、二氧化硅、碳化硅和氧化铝)组成的糊剂，该糊剂例如，在灼烧时形成堇青石。粘土或水溶性粘合剂一般用于制备足够塑性以形成可使用蜂窝体的糊剂。在挤出糊剂之后，将蜂窝体干燥，脱粘合剂和烧结以形成蜂窝体。典型地烧结蜂窝体以向薄的通道壁提供足够的强度，以保证陶瓷糊剂的***以堵塞通道，如下所述。
最后，为制造壁流颗粒捕集器或过滤器，采用包括合适粉末，分散介质和粘合剂组成的糊剂，堵塞烧结的蜂窝体一端的一半开口。然后在另一端，采用糊剂堵塞没有堵塞的通道。随后，再次烧结堵塞的蜂窝体以形成壁流颗粒捕集器。
令人遗憾地，此方法具有许多问题。例如，糊剂中的液体可优选被拉入灼烧过的蜂窝体的多孔壁中，引起栓塞的非均匀干燥收缩并导致最后栓塞中的裂纹。第二个问题是必须采用多个昂贵步骤(例如至少两个高温灼烧)以制造颗粒捕集器。由于陶瓷蜂窝体生坯(green)的壁较薄和脆，当***糊剂时，它们倾向于变形和/或断裂，因此典型地需要这多个步骤。当使用大规模方法时，这是特别真实的。另一个问题是由于在栓塞烧结收缩期间灼烧过的蜂窝体的膨胀，可用于栓塞的组成有限。
因此，需要提供一种制造壁流捕集器的方法，该方法例如避免现有技术的一个或多个问题，如上述那些的一个。
发明内容
本发明是一种堵塞陶瓷蜂窝体中通道的方法，其包括：
(a)形成包括分散液体和陶瓷粉末的混合物，
(b)在未堵塞的陶瓷蜂窝体中的通道的一端***所述混合物，使得混合物流到另一端，其中混合物收集和形成堵塞的陶瓷蜂窝体和
(c)加热堵塞的陶瓷蜂窝体到足以烧结堵塞的陶瓷蜂窝体的温度，以形成多孔的烧结的堵塞的陶瓷蜂窝体。
在本发明的一个实施方案中，优选分散液体是水或醇，更优选分散液体是甲醇、丙醇、乙醇或其混合物，最优选所述分散液体是丙醇。
在本发明的另一个实施方案中，其中***所述混合物由如下方式进行：在陶瓷蜂窝体生坯中的通道的一端***所述混合物并允许该混合物流向封闭的另一端，使得该混合物聚集和形成栓塞。优选其中另一端由多孔体封闭，该多孔体能够除去混合物的分散液体。还优选当它流过通道时，所述混合物在所述通道的壁上沉积陶瓷粉末，使得在步骤(c)加热时，在所述通道壁上形成区别层。
在本发明的另一个实施方案中，所述混合物包含催化剂。方法特别用于，但不限于蜂窝壁流过滤器中通道的堵塞。令人惊奇地，这些方法不仅仅可用于堵塞通道，而且可同时例如在陶瓷蜂窝壁流过滤器出口通道的壁上提供区别层。该方法也可用于在通道的过滤器壁之上或之中提供其它有用的材料(例如，催化剂或成核剂)，而同时形成栓塞。
附图说明
图1是显示根据本发明制造的陶瓷蜂窝过滤器一个实施方案的前视图。
图2是一部分切掉的图1的侧视图。
图3是图1过滤器中相邻通道的放大示意图。
图4是图1的通道堵塞部分和原位形成区别层的放大截面图。
在整个附图的不同视图中，数字2是陶瓷蜂窝体，数字4是入口通道，数字5是出口通道，数字6是在相邻通道之间的分配壁，数字8是入口栓塞，数字9是出口栓塞，数字10是入口端，数字11是出口端和数字12是区别层。
未堵塞的陶瓷蜂窝体：
未堵塞的陶瓷蜂窝体是含有至少一个未堵塞的通道的陶瓷蜂窝体。作为说明，该蜂窝体可含有一半在一端堵塞和在另一端无栓塞的通道(即，一半通道是未堵塞的)。
未堵塞陶瓷蜂窝体可以是生坯(green)、煅烧的或烧结的，但优选是生坯或煅烧的。未堵塞陶瓷蜂窝体生坯包括陶瓷粉末和有机粘合剂。有机粘合剂包括如在如下文献中描述的那些：
陶瓷加工原理的介绍，J.Reed，John Wiley and Sons，NY，NY，1988的11章。煅烧的未堵塞陶瓷蜂窝体是已经加热到煅烧温度的未堵塞陶瓷蜂窝体生坯，煅烧温度足以除去有机粘合剂和将可能存在的任何粘土脱水。烧结的未堵塞陶瓷蜂窝体是已经加热到烧结温度的未堵塞陶瓷蜂窝体生坯或煅烧的未堵塞陶瓷蜂窝体，烧结温度足以熔合(烧结)陶瓷组分成整体陶瓷。
堵塞的陶瓷蜂窝体：
堵塞的陶瓷蜂窝体是任何上述的未堵塞陶瓷蜂窝体，该蜂窝体的至少一个通道被混合物堵塞，混合物在加热到烧结温度时形成烧结的陶瓷栓塞，因此形成烧结的堵塞的陶瓷蜂窝体。
烧结的堵塞的陶瓷蜂窝体：
把堵塞的陶瓷蜂窝体加热到烧结温度，烧结温度足以熔合(烧结)栓塞的陶瓷组分和，如必须，陶瓷蜂窝体以形成整体陶瓷。
参考图1-图4，它表示陶瓷蜂窝过滤器的一个优选实施方案，该过滤器包括陶瓷蜂窝体2，该蜂窝体分别含有多数通过其间(即从入口端10到出口端11)延伸的多个平行入口和出口通道4和5，入口和出口通道由多孔分配壁6，入口通道栓塞8和出口通道栓塞9确定。出口通道9也含有位于分配壁6表面上的区别层12。当将包含要过滤的物质的气体或液体14导引入入口通道4时，气体或液体14通过分配壁6和区别层12并离开出口通道5。因此，分配壁6和区别层12从气体或液体14过滤出该物质。
陶瓷蜂窝体2可以是具有足够孔隙率和强度以作为壁流过滤器进行操作的任何有用陶瓷。有用陶瓷的例子包括碳化硅、氮化硅、莫来石、堇青石、β锂辉石、磷酸盐陶瓷(例如磷酸锆)或其结合物。优选，陶瓷是莫来石、碳化硅或堇青石。更优选，陶瓷是莫来石或碳化硅。优选莫来石在氟气体存在下形成，如在U.S.专利4,910,172、4,911,902、4,948,766、5,098,455、5,173,349、5,194,154、5,198,007、5,252,272和5,340,516中描述的那些。莫来石颗粒的平均长宽比优选至少为2，更优选至少5，和最优选至少10。
一般情况下，陶瓷蜂窝体2的孔隙率是30％-80％多孔的。优选，陶瓷蜂窝体2是40％-70％多孔的。栓塞8和9可以为足以有效作为栓塞的任何孔隙率。一般情况下栓塞8和9可以是包括基本与陶瓷蜂窝体2相同陶瓷组成的陶瓷组合物。基本相同的组成表示栓塞8和/或9的化学和微结构与陶瓷蜂窝体2基本相同。栓塞组合物的例子包括与先前所述用于陶瓷蜂窝体2相同的陶瓷。
在陶瓷壁流过滤器的一个优选实施方案中，栓塞8和9的组成与陶瓷蜂窝体2相同。在此实施方案中，可以存在或可以不存在区别层12。优选，存在化学与陶瓷蜂窝体基本相同的区别层12。
在另一个优选的实施方案中，烧结的陶瓷蜂窝体2在出口端11含有入口栓塞8，入口栓塞8的组成不同于在入口端10的出口栓塞9。不同的组成表示，在烧结之后，根据表征陶瓷的典型采用的技术，组合物具有容易识别的微结构差异(例如孔隙率，结晶结构或晶粒大小)或化学差异。基本意思是差异不容易由上述技术识别。优选，在一端堵塞蜂窝体2所有通道的一半(即入口通道4)和在另一端堵塞不在那一端堵塞的剩余通道(即，在入口端堵塞出口通道5)。甚至更优选，与入口栓塞8相比，出口栓塞9具有基本相同的化学但不同的微结构。进一步优选此实施方案也含有区别层12。最优选，出口栓塞9的组成与区别层12基本相同和入口栓塞8的组成与陶瓷蜂窝体2基本相同。
区别层12可以是用于制造过滤器的任何材料，只要区别层12的平均孔径大小基本小于陶瓷蜂窝体的平均孔径大小。合适的材料包括对于陶瓷蜂窝体描述的那些。“基本更小”一般表示区别层平均孔径大小至多是陶瓷蜂窝体平均孔径大小的四分之三。优选，区别层12的平均孔径大小至多是陶瓷蜂窝体2平均孔径大小的一半，更优选至多四分之一。
此外，陶瓷蜂窝壁流过滤器1可在至少一个分配壁6或区别层12之上或之中含有催化剂。催化剂可以适于催化，例如，烟煤粒子燃烧或CO(一氧化碳)或NOx(氮的氧化物)氧化的任何催化剂。例示的催化剂包括如下物质。
第一种例示催化剂是直接结合金属催化剂，如贵金属、基底金属及其结合物。贵金属催化剂的例子包括铂、铑、钯、钌、铼、银及其合金。基底金属催化剂的例子包括铜、铬、铁、钴、镍、锌、锰、钒、钛、钪及其结合物。金属催化剂的形式优选为金属，但可以存在为无机化合物，如氧化物、氮化物和碳化物，或存在为多孔催化剂载体的陶瓷晶粒中的缺陷结构。可以由任何合适的技术，如本领域已知的那些来使用该金属。例如，可以由化学气相沉积应用金属催化剂。
第二种例示催化剂是引入到前述催化剂蜂窝体的陶瓷晶粒的点阵结构的催化剂。例如，元素可以是Ce、Zr、La、Mg、Ca、先前段落中描述的金属元素或其结合物。可以采用任何合适的方式，如本领域已知的那些引入这些元素。
第三种例示催化剂是含有在其上沉积的金属的陶瓷粒子的结合物。这些物质典型地称为修补基面涂层(wash-coat)。一般情况下，修补基面涂层由含有在其上沉积的金属的微米级陶瓷粒子，如沸石、硅铝酸盐、二氧化硅、铈土、氧化锆、氧化钡、碳酸钡和氧化铝粒子组成。金属可以是先前对于直接沉积金属所述的任何金属。特别优选的修补基面涂层催化剂涂料是包括其上含有贵金属的氧化铝粒子的涂料。理解修补基面涂层可以包括多于一种金属氧化物，如氧化铝，其含有至少一种如下金属的氧化物：锆、钡、镧、镁和铈。
第四种例示催化剂是包括金属氧化物组合物的钙钛矿类型催化剂，如由Golden在U.S.专利No.5,939,354中描述的那些。
第五种例示催化剂是由一种组合物形成且沉积在在300℃-3000℃的温度下煅烧而形成的催化剂载体上，组合物包括(a)包含至少一种金属盐的盐水溶液和(b)两亲含环氧乙烷的共聚物，其中所述共聚物的平均分子量大于400，环氧乙烷含量为5-90％和HLB为-15～15，如由Gruenbauer等人的PCT专利申请No.WO99/18809所述。此外，催化剂也可以是由U.S.专利No.5,698,483和PCT专利申请No.WO99/03627描述的催化剂。
在进行堵塞陶瓷蜂窝体中通道的方法中，形成包括分散液体和陶瓷粉末的混合物。然后将该混合物***未堵塞的陶瓷蜂窝体的至少一个通道，使得混合物流到另一端，在那里混合物聚集和形成堵塞的陶瓷蜂窝体。然后加热堵塞的陶瓷蜂窝体到足以烧结栓塞和熔合它们到陶瓷蜂窝体和，如必须，也烧结陶瓷蜂窝体(即，如果它是陶瓷蜂窝体生坯或煅烧的陶瓷蜂窝体)。换言之，充分加热堵塞的陶瓷蜂窝体，以形成多孔的烧结的堵塞的陶瓷蜂窝体。
混合物必须是例如，仅从重力的施加，足以***陶瓷蜂窝体生坯通道的一端和随后流过通道和在通道的另一端聚集的流体。因此，该混合物可以在分配壁上沉积例如区分层和形成入口和出口栓塞，在除去足够量分散液体之后，以向聚集的混合物提供足够的整体性以形成栓塞。一般情况下，混合物的粘度至多为1000厘泊(cp)，更优选混合物的粘度至多为200cp，甚至更优选至多100cp和最优选至多20cp。
可以由任何合适的方法，如本领域已知的那些形成该混合物。合适的方法包括在如下文献中描述的那些：
陶瓷加工原理的介绍，J.Reed，John Wiley and Sons，NY，1988的17章。
分散液体可以是，例如，水、任何有机液体，如醇、脂族化合物、二醇、酮、醚、醛、酯、芳族化合物、烯烃、炔烃、羧酸、羧酸酰氯、酰胺、胺、腈、硝基化合物、硫化物、亚砜、砜、有机金属化合物或其混合物。优选，分散液体是水、脂族化合物、烯烃或醇。更优选，该液体是醇。优选，醇是甲醇、丙醇、乙醇或其结合物。最优选，醇是丙醇。
陶瓷粉末可以是用于形成栓塞的任何陶瓷粉末，如形成陶瓷的陶瓷粉末，如碳化硅、氮化硅、莫来石、堇青石、β锂辉石、磷酸盐陶瓷(例如磷酸锆)或其结合物。优选，陶瓷粉末形成莫来石或堇青石。陶瓷的优选例子包括二氧化硅、碳化硅、氧化铝、氟化铝、粘土、氟黄玉(fluorotopaz)、沸石、及其混合物。更优选，陶瓷粉末包括在如下方法中形成氟黄玉和莫来石的粉末：在该方法的一些时间中存在有氟气体，如先前所述。
该混合物可包含其它有用的组分，如制备陶瓷悬浮液领域中已知的那些。其它有用组分的例子包括分散剂，抗絮凝剂，絮凝剂，增塑剂，消泡剂，润滑剂和防腐剂，如在如下文献中描述的那些：
陶瓷加 工原理的介绍，J.Reed，John Wiley and Sons，NY，1988的10-12章。混合物中的优选粘合剂是溶于分散液体，但不溶于水的粘合剂。
该混合物也可包含粘合剂。粘合剂的例子包括纤维素酯，例如下文献中描述的那些：
陶瓷加工原理的介绍，J.Reed，John Wiley andSons，NY，NY，1988的11章。优选，粘合剂是甲基纤维素或乙基纤维素，如以商标METHOCEL和ETHOCEL购自The Dow ChemicalCompany的那些。优选，该粘合剂溶于分散液体，但不溶于水，如ETHOCEL。
在形成混合物之后，将它***未堵塞的陶瓷蜂窝体的通道中以形成栓塞(即，形成堵塞的陶瓷蜂窝体)。向通道中的***可以由任何合适的方法，如本领域已知的那些完成。例如，可以将混合物倾入、喷入、注入通道。
可以由任何合适的方法除去分散液体，如由在空气中干燥、通过热量或真空的施加而干燥、或在陶瓷蜂窝体一端由多孔介质封闭通道端而除去，该多孔介质由毛细管作用除去分散液体这样多孔介质的例子是熟石膏，如用于滑移浇铸陶瓷的熟石膏。特别优选密封要堵塞的通道，使得当在一端将混合物倾入所有的通道时，流体流过所有的通道和仅在另一端的密封通道处聚集以形成栓塞，而不密封的通道允许混合物离开而不形成栓塞。
在另一个优选的实施方案中，未堵塞的陶瓷蜂窝体含有至少一个在一端通道中的栓塞和至少一个不含有栓塞的通道(即开放通道)。随后，将混合物***开放通道。在栓塞在堵塞通道中的相同端，将混合物***开放通道，使得混合物沿开放通道向下流动和在开放通道中，在蜂窝体另一端形成栓塞。
在混合物的***(即，堵塞的陶瓷蜂窝体的形成)之后，将堵塞的陶瓷蜂窝体加热到足以烧结栓塞和，如必须，烧结陶瓷蜂窝体的烧结温度，以形成堵塞的烧结的陶瓷蜂窝体。一般情况下，堵塞的烧结的陶瓷蜂窝体是30％-80％多孔的，优选40％-70％多孔的。
烧结温度依赖于要形成的陶瓷，但一般情况下至少为900℃。优选，烧结温度至少为1000℃和，更优选至少1100℃到优选至多2200℃，更优选至多1750℃和最优选至多1400℃。
可以采用任何合适的方式或加热设备和在任何合适的气氛或气氛结合下，如制备所需特定烧结陶瓷领域中已知的那些，进行加热到烧结温度。
在进行方法中，可以使用已经煅烧的未堵塞的陶瓷蜂窝体。一般情况下，煅烧温度不足以基本烧结陶瓷蜂窝体生坯，但足以除去任何有机粘合剂和将任何粘土脱水，使得脱水的粘土当与水接触时基本不能再水合。
煅烧温度可以是适于基本除去任何有机粘合剂或将蜂窝体中存在的任何粘土脱水的任何温度。一般情况下，如果有存在的粘土，温度应当足够引起粘土基本不能再水合。“基本不能再水合”一般是当放入水中24小时时，90wt％的粘土不能再水合。优选，煅烧温度足够大使得当放入水中时，99％和更优选，所有的脱水粘土不能再水合。
一般情况下，煅烧温度是从400℃到至多1000℃。更优选，煅烧温度至少是500，更优选至少600，最优选至少650到优选至多950，更优选至多900，和最优选至多850℃。
煅烧气氛可以是适于将粘土脱水的任何气氛或两者。例子包括空气、真空、惰性气氛(例如，希有气体)、氮气或其结合物。用于加热到煅烧温度的方法和设备可以是任何合适的设备，如本领域已知的那些。
然后以先前所述的相同方式烧结堵塞的煅烧的陶瓷蜂窝体以形成烧结的堵塞陶瓷蜂窝体。
最后，也可以使用未堵塞的烧结的陶瓷蜂窝体。可以由任何合适的方法制备未堵塞的烧结的陶瓷蜂窝体。例如，烧结可以与对于烧结栓塞所述的相同。在***栓塞之后，如先前所述烧结栓塞以形成多孔的烧结的堵塞的陶瓷蜂窝体。
实施例
实施例1
在Adanced Ceramics Incorporated(Atlanta，GA)上，通过挤出和干燥氧化铝，粘土，粘合剂和水的糊剂混合物制备每cm2有37.2个泡孔的蜂窝体生坯。将蜂窝体生坯切割成150mm的长度。采用用于制备蜂窝体的相同糊剂混合物堵塞蜂窝体生坯一端的一半通道，以在此端(第一堵塞端)形成栓塞的方格图案。将蜂窝体放入夹具中，并使第一堵塞端向上(即，另一端或第二端向下)。
将平均粒子尺寸为3微米的莫来石粉末(Baikalox MULCR，Baikowski International Charlotte，NC)与2丙醇和3wt％乙基纤维素(ETHOCEL，The Dow Chemical，Midland，MI)混合，以形成含有10wt％莫来石的淤浆。该淤浆是流体和容易倾注。然后将该淤浆倾入第一堵塞端的未堵塞通道。该淤浆流入通道和向下流动，涂敷通道的壁和在蜂窝体另一端聚集。由于在第一堵塞端中未堵塞的通道中的毛细管作用，淤浆在第二端聚集和形成栓塞的方格图象，以形成堵塞的蜂窝过滤器生坯。
在干燥之后，将堵塞的蜂窝过滤器生坯加热到1000℃以除去粘合剂和轻微烧结氧化物。然后使用由Moyer等人的U.S.专利No.5,198,007描述的方法，将轻微烧结的蜂窝体转化成针形莫来石。获得的蜂窝壁流过滤器含有莫来石细针的区分层，其中莫来石淤浆接触蜂窝体的壁。在第一端的栓塞的莫来石微结构与蜂窝体基本相同，而第二端的栓塞的莫来石微结构类似于区分层。
实施例2
由以上相同的方法制备在一端堵塞的蜂窝体生坯。将在一端堵塞的蜂窝体生坯加热到1000℃以除去粘合剂和轻微烧结氧化物。
将实施例1的相同莫来石粉末与4wt％的METHOCEL在水中的溶液混合，以形成含有10wt％莫来石的淤浆。以与实施例1相同的方式，将淤浆向下倾入第一端的开放通道，以在第二端形成栓塞。在干燥之后，将蜂窝体加热到600℃以从在第二端的栓塞除去METHOCEL粘合剂。在此之后，使用由Moyer等人的U.S.专利No.5,198,007描述的方法，将堵塞的蜂窝体转化成针形莫来石。获得的蜂窝壁流过滤器具有与实施例1中过滤器基本相同的微结构特性。
Claims (8)
1.一种堵塞陶瓷蜂窝体中通道的方法，其包括：
(a)形成包括分散液体和陶瓷粉末的混合物，
(b)在未堵塞的陶瓷蜂窝体中的通道的一端***所述混合物，使得该混合物流到另一端，在那里混合物聚集和形成堵塞的陶瓷蜂窝体和
(c)加热所述堵塞的陶瓷蜂窝体到足以烧结所述堵塞的陶瓷蜂窝体的温度，以形成多孔的烧结的堵塞的陶瓷蜂窝体。
2.根据权利要求1所述的方法，其中所述分散液体是水或醇。
3.根据权利要求2所述的方法，其中所述分散液体是甲醇、丙醇、乙醇或其混合物。
4.根据权利要求3所述的方法，其中所述分散液体是丙醇。
5.根据权利要求1所述的方法，其中***所述混合物由如下方式进行：在陶瓷蜂窝体生坯中的通道的一端***所述混合物并允许该混合物流向封闭的另一端，使得该混合物聚集和形成栓塞。
6.根据权利要求5所述的方法，其中另一端由多孔体封闭，该多孔体能够除去混合物的分散液体。
7.根据权利要求5的方法，其中当它流过通道时，所述混合物在所述通道的壁上沉积陶瓷粉末，使得在步骤(c)加热时，在所述通道壁上形成区别层。
8.根据权利要求1所述的方法，其中所述混合物包含催化剂。
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-
2002
- 2002-04-23 WO PCT/US2002/012865 patent/WO2002085482A2/en active IP Right Grant
- 2002-04-23 AT AT02725789T patent/ATE332883T1/de not_active IP Right Cessation
- 2002-04-23 CA CA2445107A patent/CA2445107C/en not_active Expired - Fee Related
- 2002-04-23 BR BRPI0209230-1A patent/BR0209230B1/pt not_active IP Right Cessation
- 2002-04-23 AU AU2002256336A patent/AU2002256336A1/en not_active Abandoned
- 2002-04-23 ES ES02725789T patent/ES2264479T3/es not_active Expired - Lifetime
- 2002-04-23 KR KR1020037013845A patent/KR100848795B1/ko active IP Right Grant
- 2002-04-23 US US10/131,652 patent/US6803015B2/en not_active Expired - Lifetime
- 2002-04-23 CN CNB028103351A patent/CN1229307C/zh not_active Expired - Fee Related
- 2002-04-23 DE DE60213082T patent/DE60213082T2/de not_active Expired - Lifetime
- 2002-04-23 PL PL02366537A patent/PL366537A1/xx unknown
- 2002-04-23 JP JP2002583053A patent/JP3954501B2/ja not_active Expired - Fee Related
- 2002-04-23 EP EP02725789A patent/EP1385803B1/en not_active Expired - Lifetime
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| ES2264479T3 (es) | 2007-01-01 |
| BR0209230B1 (pt) | 2010-08-10 |
| US20020175451A1 (en) | 2002-11-28 |
| DE60213082D1 (de) | 2006-08-24 |
| US6803015B2 (en) | 2004-10-12 |
| KR100848795B1 (ko) | 2008-07-28 |
| DE60213082T2 (de) | 2007-01-18 |
| WO2002085482A2 (en) | 2002-10-31 |
| CA2445107A1 (en) | 2002-10-31 |
| BR0209230A (pt) | 2004-07-20 |
| ATE332883T1 (de) | 2006-08-15 |
| CA2445107C (en) | 2010-04-20 |
| PL366537A1 (en) | 2005-02-07 |
| WO2002085482A3 (en) | 2003-04-17 |
| JP2004536692A (ja) | 2004-12-09 |
| CN1511125A (zh) | 2004-07-07 |
| EP1385803B1 (en) | 2006-07-12 |
| EP1385803A2 (en) | 2004-02-04 |
| JP3954501B2 (ja) | 2007-08-08 |
| KR20040023793A (ko) | 2004-03-19 |
| AU2002256336A1 (en) | 2002-11-05 |
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