CN1512972A - 壁流整体过滤器的制造方法 - Google Patents
壁流整体过滤器的制造方法 Download PDFInfo
- Publication number
- CN1512972A CN1512972A CNA028109686A CN02810968A CN1512972A CN 1512972 A CN1512972 A CN 1512972A CN A028109686 A CNA028109686 A CN A028109686A CN 02810968 A CN02810968 A CN 02810968A CN 1512972 A CN1512972 A CN 1512972A
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- Prior art keywords
- ceramic
- ceramic honeycomb
- embolism
- honeycomb body
- mixture
- Prior art date
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
- B01D46/2418—Honeycomb filters
- B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
- B01D46/2476—Monolithic structures
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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
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Abstract
由包括如下步骤的方法,通过堵塞包括粘土的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,向包括粘土的陶瓷蜂窝体生坯的至少一个通道中***该混合物,以形成堵塞的陶瓷蜂窝体生坯,其中所述分散液体基本不能溶胀粘土。或者,将该混合物***煅烧的陶瓷蜂窝体以形成堵塞的煅烧的陶瓷蜂窝体。最后,将堵塞的陶瓷蜂窝体生坯或煅烧的陶瓷蜂窝体加热到足以烧结堵塞的陶瓷蜂窝体生坯的温度,以形成多孔的烧结的堵塞的陶瓷蜂窝体。该方法特别用于同时在通道中制造栓塞和区别层。具体而言该方法用于制造壁流过滤器,该过滤器在至少一端含有组成与区别层相同的栓塞或在每一端含有不同组成的栓塞。
Description
本申请要求2001年4月24日提交的U.S.临时申请系列No.60/285,810的权益。
本发明涉及陶瓷壁流整体过滤器及其制造方法。具体而言,本发明涉及粒子捕集器,如柴油粒子捕集器。
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***中的粒子捕集器。
如在U.S.专利No.4,276,071中描述的蜂窝陶瓷壁流通过滤器,是粒子捕集器的优选类型。这些蜂窝过滤器由如下方式制造:挤出包括水,粘合剂和陶瓷粉末(例如粘土、莫来石、二氧化硅和氧化铝)的糊剂,该糊剂例如,在灼烧时形成堇青石。粘土一般用于使糊剂具有足够塑性以形成可使用蜂窝体。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,为制造壁流粒子捕集器或过滤器,采用包括合适粉末,分散介质和粘合剂的糊剂,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粒子捕集器。
令人遗憾地,此方法具有许多问题。例如,糊剂中的液体可优先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)以制造粒子捕集器。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,例如其避免现有技术的一个或多个问题,如上述那些的一个。
本发明的第一方面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)向包括粘土的陶瓷蜂窝体生坯的至少一个通道中***该混合物,以形成堵塞的陶瓷蜂窝体生坯,其中分散液体基本不能溶胀粘土,和
(c)加热堵塞的陶瓷蜂窝体生坯到足以烧结堵塞的陶瓷蜂窝体生坯的温度,以形成多孔的烧结的堵塞的陶瓷蜂窝体。
本发明的第二方面是一种堵塞陶瓷蜂窝体中通道的方法,其包括:
(a)加热包括粘土的陶瓷蜂窝体生坯到第一温度,第一温度不足以基本烧结该陶瓷蜂窝体生坯,但足以除去粘合剂和将粘土脱水,使得脱水的粘土当与水接触时基本不能再水合,以形成煅烧的陶瓷蜂窝体,
(b)向煅烧的陶瓷蜂窝体的至少一个通道中***包括陶瓷粉末和分散液体的混合物,以形成堵塞的煅烧的陶瓷蜂窝体,和
(c)加热堵塞的煅烧的陶瓷蜂窝体到足以形成烧结的堵塞的蜂窝体的温度。
本发明的第三方面是一种包括整体陶瓷蜂窝体的陶瓷蜂窝壁流过滤器,该陶瓷蜂窝体含有由相邻入口和出口通道连接的入口端和出口端,该入口和出口通道从陶瓷体的入口端向出口端延伸,入口和出口通道由在入口和出口通道之间的多个交织薄气体过滤多孔分配壁确定和由陶瓷栓塞确定,使得入口通道在陶瓷体的出口端含有入口陶瓷栓塞和出口通道在陶瓷体的入口端含有出口陶瓷栓塞,使得当进入入口端时,流体必须通过分配壁以离开出口端,其中该陶瓷蜂窝体在出口通道的至少一个分配壁上含有区别层,区别层的组成与出口通道的出口陶瓷栓塞基本相同。
本发明的第四方面是一种包括整体陶瓷蜂窝体的陶瓷蜂窝壁流过滤器,该整体陶瓷蜂窝体含有由相邻入口和出口通道连接的入口端和出口端,该入口和出口通道从陶瓷体的入口端向出口端延伸,入口和出口通道由在入口和出口通道之间的多个交织薄气体过滤多孔分配壁确定和由陶瓷栓塞确定,使得该入口通道在陶瓷体的出口端含有入口陶瓷栓塞和出口通道在陶瓷体的入口端含有出口陶瓷栓塞,使得当进入入口端时,流体必须通过分配壁以离开出口端,其中出口陶瓷栓塞的组成不同于入口陶瓷栓塞。
每一种上述方法特别用于,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,而且可同时提供区别层,例如在陶瓷蜂窝壁流过滤器出口通道的壁上。该方法也可用于在过滤器通道的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。
图1是显示本发明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通道堵塞部分和原位形成的区别层的放大截面图。
在整个附图的视图中,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。
陶瓷蜂窝体生坯:
包括粘土和,如果必须,其它陶瓷的蜂窝体。粘土是溶胀和吸收水以形成塑性本体的层状水合硅铝酸盐。粘土矿物质的例子包括高岭石、蒙脱石、绿坡缕石(atapulgite)、伊利石、膨润土、多水高岭土、叶蜡石和云母。
煅烧的陶瓷蜂窝体:
已经加热到煅烧温度的陶瓷蜂窝体生坯,煅烧温度足以将陶瓷蜂窝体生坯中存在的粘土脱水,但不足以基本烧结蜂窝体的陶瓷组分。
堵塞的陶瓷蜂窝体生坯或煅烧的堵塞的陶瓷蜂窝体:
已经由混合物堵塞至少一个通道的陶瓷蜂窝体生坯或煅烧的陶瓷蜂窝体,在加热以形成烧结的堵塞的陶瓷蜂窝体时,混合物形成陶瓷栓塞。
烧结的堵塞的陶瓷蜂窝体:
加热到烧结温度的堵塞的陶瓷蜂窝体生坯或煅烧的堵塞的陶瓷蜂窝体,烧结温度足以熔合(烧结)陶瓷组分成整体陶瓷。
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,该蜂窝体分别含有分别通过其间(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和离开出口通道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,陶瓷是莫来石或堇青石。更优选,陶瓷是莫来石。最优选,陶瓷是在氟气体存在下形成的莫来石,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,由表征陶瓷典型采用的技术,该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。基本相同是当差异不容易由上述技术识别时。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和更优选,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使用该金属。例如,可以由化学气相沉积提供金属催化剂。
第二种例示催化剂是引入到前述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-coats)。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在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,如含有至少一种如下金属的氧化物的氧化铝: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等人在PCT专利申请No.WO99/18809所述。此外,该催化剂也可以是由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第一优选方法中,形成包括分散液体和陶瓷粉末的混合物。然后将该混合物***陶瓷蜂窝体生坯的至少一个通道以形成堵塞的陶瓷蜂窝体生坯,其中所述分散液体基本不能溶胀粘土。然后将堵塞的陶瓷蜂窝体生坯加热到足以烧结堵塞的陶瓷蜂窝体生坯的温度,以形成多孔的烧结的堵塞的陶瓷蜂窝体。
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。
在此方法中,分散液体必须是基本不能溶胀陶瓷蜂窝体生坯中粘土的液体。“基本不能溶胀粘土”表示分散液体不能溶胀粘土到足以引起陶瓷生坯的分配壁变形或断裂。一般情况下,基本不能溶胀是当粘土不能吸收多于1体积%的分散液体时。由于粘土不利地受水影响,分散液体应当具有不足以引起上述溶胀的水浓度。一般情况下,水的数量应当小于5体积%的分散液体。
依赖于烧结的堵塞的陶瓷蜂窝体中所需的最终陶瓷,陶瓷蜂窝体生坯中的粘土数量可在宽范围内变化。一般情况下,粘土的数量应当是足以挤出陶瓷蜂窝体生坯的数量。典型地,粘土的数量是陶瓷蜂窝体生坯的至少1体积%。
分散液体可以是,例如,不溶胀粘土的任何有机液体,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(carboxylic acid chloride)、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,如上所述。优选,分散液体是脂族化合物、烯烃或醇。更优选,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、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,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。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 Chemical Company的那些。优选,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***陶瓷蜂窝体生坯的通道中以形成栓塞(即,形成堵塞的陶瓷蜂窝体生坯)。向通道中***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、压挤入(squeezed)、挤出(extruded)或捏合入通道。
在优选的实施方案中,该混合物是例如,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,例如混合物可以在分配壁上沉积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,以向收集的混合物提供足够的整体性以形成栓塞。在此优选的实施方案中,混合物的粘度优选至多为1000厘泊(cp),更优选至多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它,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收集以形成栓塞,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生坯加热到足以烧结堵塞的陶瓷蜂窝体生坯的烧结温度,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%多孔的和优选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2000℃,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结合气氛下,如制备所需特定烧结的陶瓷领域中已知的那些,进行加热到烧结温度。
在形成堵塞的烧结的陶瓷蜂窝体的另一种方法中,将陶瓷蜂窝体生坯加热到煅烧温度,该煅烧温度不足以基本烧结陶瓷蜂窝体生坯,但足以将粘土脱水,使得脱水的粘土当与水接触时基本不能再水合,以形成煅烧的陶瓷蜂窝体。
煅烧温度可以是适于基本将粘土脱水,使得粘土基本不能再水合的任何温度。“基本不能再水合”一般是当放入水中24小时时,如果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。
在煅烧之后,如先前所述将该混合物***通道,以形成堵塞的煅烧的陶瓷蜂窝体。在此方法中,分散液体可以是水。这样的原因是由于煅烧的陶瓷蜂窝体并不包含足够可再水合(即溶胀)的粘土,以引起煅烧的陶瓷蜂窝体分配壁的有害断裂。
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。将该蜂窝体生坯切割成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)。
将平均粒子大小为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。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,淤浆在第二端收集和形成栓塞的方格图案,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等人在U.S.专利No.5,198,007中描述的方法,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。以实施例1的相同方式,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等人在U.S.专利No.5,198,007中描述的方法,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 (25)
1.一种堵塞陶瓷蜂窝体中通道的方法,其包括以下步骤:
(a)形成包括分散液体和陶瓷粉末的混合物,
(b)向包括粘土的的陶瓷蜂窝体生坯的至少一个通道中***所述混合物,以形成堵塞的陶瓷蜂窝体生坯,其中所述分散液体基本不能溶胀所述粘土,和
(c)加热所述的堵塞的陶瓷蜂窝体生坯到足以烧结该堵塞的陶瓷蜂窝体生坯的温度,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,使得所述混合物聚集和形成栓塞。
6.根据权利要求5所述的方法,其中所述另一端由多孔体封闭,该多孔体能够除去所述混合物的分散液体。
7.根据权利要求5所述的方法,其中当其流过所述通道时,所述混合物在该通道壁上沉积陶瓷粉末,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。
9.一种堵塞陶瓷蜂窝体中通道的方法,其包括以下步骤:
(a)加热包括粘土的陶瓷蜂窝体生坯到第一温度,第一温度不足以基本烧结所述陶瓷蜂窝体生坯,但足以除去所述粘合剂并将所述粘土脱水,使得该脱水的粘土在与水接触时不能再水合,从而形成煅烧的陶瓷蜂窝体,
(b)向所述煅烧的陶瓷蜂窝体的至少一个通道中***包括陶瓷粉末和分散液体的混合物,以形成堵塞的煅烧的陶瓷蜂窝体,和
(c)加热所述堵塞的煅烧的陶瓷蜂窝体到足以形成烧结的堵塞的蜂窝体的温度。
10.根据权利要求9所述的方法,基中所述煅烧温度是400℃-900℃和步骤(c)的温度至少为1000℃。
11.根据权利要求10所述的方法,其中所述分散液体是醇。
12.根据权利要求11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。
13.根据权利要求12所述的方法,其中所述分散液体是丙醇。
14.根据权利要求9所述的方法,其中***所述混合物由如下方式进行:在煅烧的陶瓷蜂窝体中通道的一端***所述混合物并允许该混合物流向封闭的另一端,使得所述混合物在另一端聚集和形成栓塞。
15.根据权利要求14所述的方法,其中所述另一端由多孔体封闭,该多孔体能够除去所述混合物的分散液体。
16.根据权利要求14所述的方法,其中当其流过通道时,所述混合物在所述通道壁上沉积陶瓷粉末,使得在步骤(c)加热时,在所述通道壁上形成区别层。
17.根据权利要求9所述的方法,其中所述混合物包含催化剂。
18.一种包括整体陶瓷蜂窝体的陶瓷蜂窝壁流过滤器,该陶瓷蜂窝体含有由相邻入口和出口通道连接的入口端和出口端,该入口和出口通道从所述陶瓷体的入口端向出口端延伸,所述入口和出口通道由在该入口和出口通道之间的多个交织薄气体过滤多孔分配壁确定和由陶瓷栓塞确定,使得所述入口通道在所述陶瓷体的出口端含有入口陶瓷栓塞和所述出口通道在所述陶瓷体的入口端含有出口陶瓷栓塞,使得当进入入口端时,流体必须通过分配壁以离开出口端,其中所述陶瓷蜂窝体在出口通道的至少一个分配壁上含有区别层,所述区别层的组成与所述出口通道的出口陶瓷栓塞基本相同。
19.根据权利要求18所述的陶瓷蜂窝壁流过滤器,其中所述整体陶瓷蜂窝体是莫来石和所述区别层是孔隙率比所述整体陶瓷蜂窝体的莫来石更细的莫来石。
20.根据权利要求18所述的陶瓷蜂窝壁流过滤器,其中所述入口陶瓷栓塞和整体陶瓷蜂窝体具有基本相同的组成。
21.一种包括整体陶瓷蜂窝体的陶瓷蜂窝壁流过滤器,所述陶瓷蜂窝体含有由相邻入口和出口通道连接的入口端和出口端,该入口和出口通道从所述陶瓷体的入口端向出口端延伸,所述入口和出口通道由在所述入口和出口通道之间的多个交织薄气体过滤多孔分配壁确定和由陶瓷栓塞确定,使得所述入口通道在所述陶瓷体的出口端含有入口陶瓷栓塞和所述出口通道在所述陶瓷体的入口端含有出口陶瓷栓塞,使得当进入入口端时,流体必须通过分配壁以离开所述出口端,其中所述出口陶瓷栓塞的组成不同于所述入口陶瓷栓塞。
22.根据权利要求21所述的陶瓷蜂窝壁流过滤器,其中所述陶瓷蜂窝体在所述出口通道的至少一个分配壁上含有区别层,所述区别层的组成与所述出口通道中的出口陶瓷栓塞基本相同。
23.根据权利要求22所述的陶瓷蜂窝壁流过滤器,其中所述区别层具有与所述陶瓷蜂窝体基本相同的化学,但具有与所述陶瓷蜂窝体不同的微结构。
24.根据权利要求18所述的陶瓷蜂窝壁流过滤器,其中在至少一个分配壁、入口栓塞或出口栓塞之中或之上存在催化剂。
25.根据权利要求21所述的陶瓷蜂窝壁流过滤器,其中在至少一个分配壁、入口栓塞或出口栓塞之中或之上存在催化剂。
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- 2002-04-23 DE DE60239196T patent/DE60239196D1/de not_active Expired - Lifetime
- 2002-04-23 BR BRPI0209232-8A patent/BR0209232B1/pt not_active IP Right Cessation
- 2002-04-23 KR KR1020087017372A patent/KR100908800B1/ko active IP Right Grant
- 2002-04-23 EP EP02731475A patent/EP1385805B1/en not_active Expired - Lifetime
- 2002-04-23 AT AT02731475T patent/ATE498598T1/de not_active IP Right Cessation
- 2002-04-23 JP JP2002583349A patent/JP4813756B2/ja not_active Expired - Fee Related
- 2002-04-23 KR KR1020037013855A patent/KR100879751B1/ko active IP Right Grant
- 2002-04-23 WO PCT/US2002/012866 patent/WO2002085814A2/en active Application Filing
- 2002-04-23 CN CNB028109686A patent/CN100412031C/zh not_active Expired - Fee Related
- 2002-04-23 CN CNA2007101941587A patent/CN101311501A/zh active Pending
- 2002-04-23 EP EP10155265A patent/EP2206693A1/en not_active Withdrawn
- 2002-04-23 CA CA2445079A patent/CA2445079C/en not_active Expired - Fee Related
- 2002-04-23 AU AU2002303452A patent/AU2002303452A1/en not_active Abandoned
- 2002-04-23 US US10/131,670 patent/US6840976B2/en not_active Expired - Lifetime
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CN101939073B (zh) * | 2007-10-12 | 2014-08-27 | 陶氏环球技术公司 | 耐热冲击性改进的烟灰过滤器 |
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CN102006922B (zh) * | 2008-02-14 | 2014-06-04 | 巴斯夫公司 | 具有低铂/钯比的csf |
CN112707745A (zh) * | 2013-03-15 | 2021-04-27 | 康宁股份有限公司 | 蜂窝状陶瓷制品及其制造方法 |
CN114206466A (zh) * | 2018-07-31 | 2022-03-18 | 康宁股份有限公司 | 蜂窝体及堵塞蜂窝体的方法 |
US11919194B2 (en) | 2018-07-31 | 2024-03-05 | Corning Incorporated | Methods of plugging a honeycomb body |
CN113286772A (zh) * | 2018-08-31 | 2021-08-20 | 康宁股份有限公司 | 制造具有无机过滤沉积物的蜂窝体的方法 |
CN113348156A (zh) * | 2018-09-03 | 2021-09-03 | 康宁股份有限公司 | 具有多孔材料的蜂窝体 |
CN113348156B (zh) * | 2018-09-03 | 2023-10-27 | 康宁股份有限公司 | 具有多孔材料的蜂窝体 |
CN111744372A (zh) * | 2020-07-06 | 2020-10-09 | 广州市还原科技有限公司 | 一种多孔超滤陶瓷材料、含有该材料的制品及其制备 |
CN111744372B (zh) * | 2020-07-06 | 2022-06-28 | 广州市还原科技有限公司 | 一种多孔超滤陶瓷材料、含有该材料的制品及其制备 |
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WO2002085814A3 (en) | 2003-01-03 |
AU2002303452A1 (en) | 2002-11-05 |
KR100908800B1 (ko) | 2009-07-22 |
CN100412031C (zh) | 2008-08-20 |
JP4813756B2 (ja) | 2011-11-09 |
WO2002085814A2 (en) | 2002-10-31 |
CN101311501A (zh) | 2008-11-26 |
EP2206693A1 (en) | 2010-07-14 |
BR0209232B1 (pt) | 2011-07-26 |
US20020178707A1 (en) | 2002-12-05 |
CA2445079A1 (en) | 2002-10-31 |
JP2004532145A (ja) | 2004-10-21 |
EP1385805A2 (en) | 2004-02-04 |
US6840976B2 (en) | 2005-01-11 |
KR20080087120A (ko) | 2008-09-30 |
KR100879751B1 (ko) | 2009-01-21 |
KR20040023794A (ko) | 2004-03-19 |
DE60239196D1 (de) | 2011-03-31 |
CA2445079C (en) | 2010-07-20 |
BR0209232A (pt) | 2004-07-20 |
ATE498598T1 (de) | 2011-03-15 |
PL366538A1 (en) | 2005-02-07 |
EP1385805B1 (en) | 2011-02-16 |
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