CN1925901A - 过滤器和过滤器集合体 - Google Patents
过滤器和过滤器集合体 Download PDFInfo
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- CN1925901A CN1925901A CNA2005800064572A CN200580006457A CN1925901A CN 1925901 A CN1925901 A CN 1925901A CN A2005800064572 A CNA2005800064572 A CN A2005800064572A CN 200580006457 A CN200580006457 A CN 200580006457A CN 1925901 A CN1925901 A CN 1925901A
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Abstract
本发明涉及过滤器和过滤器集合体,所述过滤器为蜂窝过滤器(10),该蜂窝过滤器(10)具有多个贯通孔(12),在该贯通孔(12)彼此之间的壁部(15)上形成有担载了催化剂的涂覆层。对于该过滤器(10),将壁部(15)上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A(%),将该壁部(15)上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B(%),将与所述贯通孔(12)垂直相交的面的开口率设为C(%)时,其满足2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20)。过滤器(10)更优选满足2.5×A/B+55.5≤C。这样,能够进一步降低压力损失。或者,更优选满足C≤2.5×A/B+58.0。这样,能够进一步提高粒状物质的捕获效率。
Description
技术领域
本发明涉及一种过滤器和过滤器集合体。
背景技术
以往,作为过滤器,已提出有根据气孔分布对贯通孔彼此之间的壁部厚度进行了改进的过滤器。例如,在日本特开2001-269522号公报中记载的过滤器,对于该过滤器,若将气孔径为30μm以上的气孔的容积相对于全部气孔容积的比例设为P1、将壁厚设为T,则P1为10%时,将壁厚T设为100μm以上,P1为30%时,将壁厚T设为300μm以上,即满足P1×10≤T。另外,若将气孔径小于3μm的气孔的容积相对于全部气孔容积的比例设为P3、将壁厚设为T,则P3为10%时,将壁厚T设为150μm以下,P3为30%时,将壁厚T设为50μm以下,即满足(1/P3)×1500≥T。这样,在过滤器中存在较多大气孔径的气孔的容积时,通过增大壁厚,来提高粒状物质的捕获效率,另一方面,存在较多小气孔径的气孔的容积时,通过减少壁厚,来减小压力损失。
但是,在该公报中所记载的过滤器中,在制作大气孔径气孔的容积较多的过滤器的情况下,将壁厚增大为满足P1×10≤T时,有时会导致压力损失增高。另外,在制作小气孔径的气孔的容积较多的过滤器的情况下,将壁厚减小为满足(1/P3)×1500≥T时,有时导致粒状物质的捕获效率降低。并且,开口率等也会影响到气体的流通,因此,仅靠调节壁厚,有时不能充分降低压力损失并捕获颗粒物质。
发明内容
本发明是鉴于上述课题提出的,其目的在于,提供一种过滤器和过滤器集合体,其能够降低压力损失并充分捕获粒状物质。
本发明为了达到上述目的,采取了如下措施。
即,本发明的过滤器是具有多个贯通孔的过滤器,
当将所述贯通孔彼此之间的壁部上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A(%),将该壁部上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B(%),将与所述贯通孔垂直相交的面的开口率设为C(%)时,满足2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20)。
通常,在这种过滤器中,贯通孔在流体(例如气体或液体等)的流入侧和流出侧的端部的某一方被封孔,将这些贯通孔彼此隔开的壁部起到过滤器的作用。即,流入贯通孔的流体通过壁部之后,从其它的贯通孔流出。此时,例如流体中含有的粒状物质等被壁部去除。此处,压力损失根据流体流入/流出过滤器时的阻抗、通过壁部时的阻抗而变化,因此,可推测出压力损失受到过滤器的开口率和壁部的气孔分布等影响。并且,粒状物质的捕获效率根据粒状物质通过壁部的难易程度等变化,因此,可推测出粒状物质的捕获效率受到过滤器的开口率和壁部的气孔分布等的影响。本发明者们,着眼于过滤器的开口率和壁部的气孔分布之间的关系,所述气孔分布是指规定气孔径的气孔相对于全部气孔容积所占的比例,进行潜心研究,结果发现当将壁部上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A(%),将该壁部上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B(%),将与所述贯通孔垂直相交的面的开口率设为C(%)时,若充分满足2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20),则能够降低压力损失并充分捕获粒状物质,从而完成了本发明。
另外,本发明的过滤器是具有多个贯通孔的过滤器,
在所述贯通孔彼此之间的壁部上担载有催化剂,
当将所述壁部上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A(%),将该壁部上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B(%),将与所述贯通孔垂直相交的面的开口率设为C(%)时,所述过滤器满足2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20)。
根据该过滤器,由于在担载了催化剂之后满足上述式,所以能够降低压力损失并充分捕获粒状物质。此处,作为催化剂,可以是有助于废气中含有的粒状物质的燃烧的催化剂、以及将废气中的CO、烃(HC)、NOx等净化的催化剂,可以是例如贵金属、碱金属和碱土金属等,也可以是氧化物等。作为贵金属,可以举出选自例如铂、钯和铑等的1种以上贵金属,作为碱金属,可以举出选自例如钠和钾等的1种以上碱金属,作为碱土金属,可以举出选自例如镁、钡等的1种以上碱土金属。并且,作为氧化物,可以举出选自例如具有钙钛矿构造的物质(LaCoO3,LaMnO3等)以及CeO2等的1种以上氧化物。作为具有钙钛矿构造的氧化物,可以举出下述物质:例如钙钛矿构造(通式ABO3)的A位置为选自La、Y以及Ce等的1种以上的元素,其中优选La,通式的B位置为选自Fe、Co、Ni和Mn等的1种或2种以上的元素。另外,也可以象La0.75K0.25CoO3那样,将A位置的元素的一部分取代为K、Sr以及Ag等。
在本发明的过滤器中,更优选满足2.5×A/B+55.5≤C。这样,能够进一步降低压力损失。
在本发明的过滤器中,更优选满足C≤2.5×A/B+58.0。这样,能够进一步提高粒状物质的捕获效率。
在本发明的过滤器中,优选所述开口率为58%以上。这是因为,开口率小于58%时,有时压力损失较大。
在本发明的过滤器中,优选所述开口率为75%以下。这是因为,开口率大于75%时,构成壁的基材减少,有时强度降低。
在本发明的过滤器中,优选所述贯通孔彼此之间的壁厚为0.15mm~0.40mm。这是因为,壁厚小于0.15mm时,有时强度降低,若大于0.40mm,则废气难以通过壁,有时压力损失增高。
在本发明的过滤器中,优选孔密度为31个/cm2~78个/cm2。这是因为,孔密度小于31个/cm2时,有时废气通过或接触的壁的面积(过滤面积)减小,若大于78个/cm2,则有时压力损失增高。
本发明的过滤器,优选主成分为选自例如碳化硅、氮化硅、氧化硅、氧化铝、氧化锆、氧化钛、氧化铈、莫来石、堇青石以及钛酸铝的1种以上物质,其中优选碳化硅。这是因为,碳化硅具有作为捕获/燃烧废气中的粒状物质的过滤器为理想的热传导率等性质。
本发明的过滤器集合体是将2个以上的过滤器(上述的任意一种过滤器)以没有所述贯通孔开口的外表面通过密封材料层接合而形成的。
在该过滤器接合体中,能够提高对热冲击和振动的强度。据推测其理为,由于在过滤器的外周存在密封材料层,所以能够通过密封材料层来缓和热冲击和振动。
附图说明
图1是本实施方式的蜂窝过滤器10的说明图。
图2是表示A/B值和开口率的优选范围的图。
图3是本实施方式的蜂窝过滤器30的说明图。
图4是本实施方式的蜂窝过滤器20的说明图。
图5是压力损失测定装置40的说明图。
图6是废气净化测定装置60的说明图。
图7是表示A/B值和开口率的关系的图。
具体实施方式
下面,利用附图,对实施本发明的优选方式进行说明。
首先,说明本实施方式的过滤器。图1是本实施方式的蜂窝过滤器10的说明图,图1(a)是立体图,图1(b)是图1(a)的X-X截面图。该蜂窝过滤器10构成为柴油微粒过滤器,其具有如下功能:将柴油发动机的废气中的粒状物质(下面称为PM)过滤,并燃烧净化。该蜂窝过滤器10具有沿长度方向并排的多个贯通孔12。该贯通孔12的端面被封孔部14交错封孔。因此,在该蜂窝过滤器10中,从贯通孔12的入口流入的废气通过壁部15流通到相邻的贯通孔12,此时,废气中含有的PM被蜂窝过滤器10的壁部15捕获。并且,在蜂窝过滤器10的壁部15上形成有涂布了催化剂载体的涂覆层,在该涂覆层上担载有催化剂。
对于该蜂窝过滤器10,当将壁部15上的气孔径为10μm以下的气孔相对于全部气孔容积所占比例设为A%(下面称为比例A),将壁部15上的气孔径为30μm以上的气孔相对于全部气孔容积所占比例设为B%(下面称为比例B),将与贯通孔12垂直相交的蜂窝过滤器10的面的开口率设为C%(下面称为比例C)时,该过滤器充分满足式(1):2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20)。此处,开口率C是指没有形成封孔部14的面(图1(b)中Y-Y截面)的开口率。并且,开口率是指在蜂窝过滤器的截面中,贯通孔的面积总和相对于蜂窝过滤器的截面积所占的比例。图2中示出比例A与比例B之比、即A/B值和开口率C的优选范围。该蜂窝过滤器10在担载了催化剂之后,充分满足式(1)。另外,在使用时不担载催化剂的情况下,需要在没有担载催化剂的状态下充分满足式(1)。并且,蜂窝过滤器10优选满足式(2):2.5×A/B+55.5≤C。在该范围内,能够进一步降低压力损失。并且,蜂窝过滤器10优选满足式(3):C≤2.5×A/B+58.0。在该范围内,能够进一步提高PM的捕获效率。该开口率C优选为58%~75%。这是因为,开口率小于58%时,有时压力损失较大,开口率大于75%时,基材减少,强度有可能降低。
该蜂窝过滤器10的气孔率优选为30%~80%,更优选为40%~60%。气孔率小于30%时,压力损失有可能增高,气孔率大于80%时,强度有可能降低。在该蜂窝过滤器10中,比例A形成为20%以下。若该比例大于20%,则气孔径较小的气孔容积的比例增大,压力损失有可能增大,所以不理想。并且,比例B形成在0%~20%(其中不包括0%)的范围内。若该比例大于20%,则气孔径较大的气孔容积的比例增大,PM的捕获效率有可能减小,所以不理想。即,为了减小压力损失并增大PM的捕获效率,优选气孔径为10μm~30μm范围的气孔容积的比例在60%以上。并且,A/B值优选为0~10(其中不包括0),更优选为3以下。并且,蜂窝过滤器10的平均气孔径优选为10μm~30μm。
形成于蜂窝过滤器10的贯通孔12彼此之间的壁部15的厚度(壁厚)优选为0.15mm~0.4mm的范围。这是因为,壁厚小于0.15mm时,有时强度降低,若大于0.4mm,则废气难以通过壁部15,有时压力损失增大。并且,每单位截面积的贯通孔12的数量(孔密度)优选为31个/cm2~78个/cm2(200cpsi~500cpsi)。这是因为,贯通孔的数量小于31个/cm2时,过滤面积减小,若大于78个/cm2,则压力损失增高,难以制作蜂窝过滤器30。另外,贯通孔12的形状可以是矩形,也可以是三角形或六边形。
蜂窝过滤器10是将碳化硅作为主成分来形成的。另外,也可以将例如氮化硅、氧化铝、氧化硅、氧化锆、堇青石、莫来石或钛酸铝等作为主成分来制作蜂窝过滤器10。
并且,蜂窝过滤器10担载有作为催化剂的贵金属铂。催化剂的担载量,优选蜂窝过滤器10的每单位体积的催化剂的重量为0.1g/L~8g/L。另外,也可以不在蜂窝过滤器10上担载催化剂,而用于PM的捕获。
接着,按照各个工序分别来说明本发明的蜂窝过滤器10的制造方法。此处,说明将碳化硅作为主成分来制造蜂窝过滤器10的方法。该碳化硅使用将规定平均粒径的粗颗粒(下面称为粗粒碳化硅)和比规定平均粒径小的平均粒径的微细颗粒(下面称为微粒碳化硅)混合而得的碳化硅。另外,微粒碳化硅使用与粗粒碳化硅的结晶方式不同的碳化硅。
在本说明书中,平均粒径是指使用MALVERN制的微粒粒径量测仪,根据激光衍射散射法来求出的值。
(1)原料混合工序
使用蜂窝过滤器的原料中含有的粗粒碳化硅的平均粒径为5μm~100μm(优选5μm~50μm)范围的粗粒碳化硅。微粒碳化硅使用平均粒径为0.1μm~5μm(优选0.1μm~3μm)的碳化硅。使用粗粒碳化硅的平均粒径为微粒碳化硅的平均粒径的5倍~100倍的碳化硅。作为原料的添加比,相对于全部的碳化硅,优选粗粒碳化硅的量为60重量%~80重量%,微粒碳化硅的量为20重量%~40重量%。
然后,相对于100质量份的上述混合了粗粒碳化硅和微粒碳化硅的碳化硅,可以添加20重量份以下的成孔剂。该成孔剂,可以举出选自例如将氧化物类陶瓷作为主成分的微小中空球体即微球(balloon)、球状丙烯酸树脂颗粒、石墨等的1种以上的材料。此处,作为氧化物的微球,可以举出选自例如氧化铝微球、玻璃微球、火山灰微球、飞灰微球(FA ballons)以及莫来石微球等的1种以上的微球。另外,成孔剂的添加量(包括添加量为0的情况),可以结合想要得到的蜂窝过滤器10的气孔率来适当选择。接着,相对于100重量份的混合了粗粒碳化硅和微粒碳化硅的碳化硅,加入10重量份~35重量份的水,做成坯土。另外,作为分散介质,除了水之外,可以举出例如有机溶剂(苯等)以及醇(甲醇等)等。除了这些以外,还可以结合成型性,在该坯土中适当添加有机粘合剂和成型助剂。作为有机粘合剂,可以举出选自例如甲基纤维素、羧甲基纤维素、羟乙基纤维素、聚乙二醇、苯酚树脂和环氧树脂的1种以上的有机粘合剂。对于有机粘合剂的添加量,相对于100重量份的混合了粗粒碳化硅和微粒碳化硅的碳化硅,优选为1重量份~12重量份。作为成型助剂,可以举出例如乙二醇、糊精、脂肪酸、脂肪酸皂和多元醇。该坯土可以使用例如搅拌机或粉碎机等进行混合,也可以使用捏和机等充分捏合。
(2)成型烧制工序
接着,将在原料混合工序中得到的、含有粗粒碳化硅和微粒碳化硅的坯土成型为蜂窝形状。对坯土进行成型的方法,可以通过挤出成型、铸造成型和冲压成型等来进行,此处通过挤出成型来进行。成型的蜂窝过滤器的形状可以是任意的形状、大小,可以是例如圆柱状、棱柱状、或椭圆柱状。此处,成型为棱柱状,该棱柱状上形成有沿长度方向并排的多个贯通孔。另外,对于开口率、壁厚以及孔密度等,可以结合使用目的在上述的范围内进行适当选择。并且,贯通孔12的形状可以是矩形,也可以是三角形或六边形。此处,在制作A/B值小的蜂窝过滤器10的情况下,大气孔多,PM的捕获效率容易降低,所以,优选在满足上述的式(1)的范围内,减小开口率C。作为减小开口率C的方法,可以举出如下方法:增大孔密度,或增大壁部15的壁厚,或增大孔密度并增大壁厚。另一方面,在制作A/B值大的蜂窝过滤器10的情况下,小气孔多,容易变得废气难以通过,所以,优选在满足上述的式(1)的范围内,增大开口率C。作为增大开口率C的方法,可以举出如下方法:减小孔密度,或减小壁厚,或减小孔密度并减小壁厚。然后,对得到的粗成型体进行干燥。干燥使用例如微波干燥机、热风干燥机等,在100℃~200℃左右的温度下进行。然后,对多个贯通孔12的各个贯通孔,利用与上述坯土的组成相同的糊仅在一方的端面形成封孔部14,进行封孔,然后再次进行干燥。具体讲,对多个贯通孔12,使得一方的端面被封孔而另一方的端面开口的贯通孔12与一方的端面开口而另一方的端面被封孔的贯通孔12交错排列。
接着,对得到的粗成型体进行烧制。在原料混合工序中添加了有机粘合剂等有机成分时,优选在烧制前进行预烧制,将该有机成分脱脂。作为预烧制条件,根据所添加的有机成分的量和种类来适当选择,例如在氧气氛下、在300℃~650℃左右进行加热。成型体的烧制在例如氮或氩等惰性气体气氛下,在1500℃~2300℃(更优选1900℃~2200℃)的条件下进行。这样,得到由碳化硅构成的蜂窝结构体(称为担载催化剂之前的蜂窝过滤器10)。
(3)催化剂担载工序
接着,在得到的蜂窝结构体上担载作为催化剂的铂。可以在壁部15上设置涂布了作为催化剂载体的氧化铝的涂覆层,在该涂覆层上担载该催化剂。作为担载方法,可以举出例如浸渍法等。另外,也可以在蜂窝过滤器10上担载被赋予了催化剂的氧化铝。首先,调制涂覆层用浆料,将蜂窝结构体浸渍于该浆料中之后,提起,通过抽吸将残留在贯通孔12等中的多余的浆料去除。然后,在80℃~200℃下进行干燥,在500℃~700℃下进行烧制,以设置涂覆层。接着,进行如下工序:将蜂窝结构体浸渍于含有催化剂的溶液中之后,进行干燥,在500℃~700℃下进行烧制,从而得到担载有铂的蜂窝过滤器10。催化剂的担载量,可以根据使用目的来适当选择,此处,将涂覆层形成为蜂窝过滤器10的每单位体积的作为催化剂载体的氧化铝达到50g/L~120g/L,蜂窝过滤器10的每单位体积的催化剂的担载量达到铂为0.1g/L~0.8g/L。另外,可以担载作为氧化催化剂的贵金属(例如钯和铑等)、作为氧化催化剂的氧化物(具有钙钛矿构造的物质(LaCoO3,LaMnO3等)以及CeO2等),也可以担载作为NOx吸收催化剂的碱金属(钾等)以及碱土类金属(钡等)等。该蜂窝过滤器10能够捕获废气中含有的PM,净化废气中含有的NOx、HC和CO。
此处是对一体成型为棱柱状的蜂窝过滤器10的制造方法进行说明的,但如图3所示,也可以是形成为圆柱状的蜂窝过滤器30。该蜂窝过滤器30利用封孔部34将贯通孔32的端部交错封孔。或者,如图4所示,也可以将该蜂窝过滤器10作为蜂窝单元11多个接合,并加工成圆柱状的蜂窝过滤器20(本发明的蜂窝集合体)。该蜂窝过滤器20具有:多个蜂窝单元11,其形成为棱柱状,具有沿长度方向并排的多个贯通孔12;密封材料层26,其将蜂窝单元11在没有贯通孔12开口的外表面13接合;以及涂覆材料层27,其覆盖由密封材料层26接合的2个以上的蜂窝单元11中没有贯通孔12开口的外周面。另外,也可以不具有涂覆材料层27。说明该蜂窝过滤器20的制造方法。首先,制造多个上述的蜂窝过滤器10,将它们作为蜂窝单元11,在蜂窝单元11的外表面13上涂布密封材料,将多个蜂窝单元11接合,在120℃对该密封材料进行干燥、固化,形成密封材料层26。此处,蜂窝单元11的总截面积相对于蜂窝过滤器20的截面积所占的比例优选为85%以上,更优选为90%以上。这是因为,该比例小于85%时,密封材料层26和涂覆材料层27等蜂窝过滤器10以外部分的截面积增大,导致压力损失增大。接着,用金刚石刀具等将该接合的过滤器切割加工成圆柱状,使用涂覆材料对没有贯通孔12开口的外周面进行涂布,在120℃进行干燥、固化,形成涂覆材料层27。接着,与上述蜂窝过滤器10同样地,可以在涂布催化剂载体之后,担载催化剂。这样,得到蜂窝过滤器20。此处,作为密封材料和涂覆材料,可以使用包括无机纤维和无机颗粒的至少一方、并在其中适当添加有无机粘合剂、有机粘合剂的材料。作为无机纤维,可以举出选自例如氧化硅一氧化铝、莫来石、氧化铝以及氧化硅的一种以上的陶瓷纤维。作为无机颗粒,可以举出选自例如碳化硅、氮化硅以及氮化硼等的1种以上的颗粒。作为无机粘合剂,可以举出选自例如氧化硅溶胶、氧化铝溶胶等的1种以上的粘合剂。作为有机粘合剂,可以举出选自例如聚乙烯醇、甲基纤维素、乙基纤维素以及羧甲基纤维素等的1种以上有机粘合剂。在该蜂窝过滤器20中,将2个以上的蜂窝过滤器10在没有贯通孔12开口的外表面13利用密封材料层26接合,所以能够提高对热冲击和振动的强度。
根据以上叙述的本实施方式的蜂窝过滤器10,由于充分满足式(1):2.5×A/B+52.5≤C≤2.5×A/B+60.2(A≤20,0<B≤20),所以能够降低压力损失并充分捕获PM。并且,由于满足2.5×A/B+55.5≤C,所以能够进一步降低压力损失。而且,由于满足C≤2.5×A/B+58.0,所以能够进一步提高PM的捕获效率。而且,开口率为58%~75%,所以压力损失不会变得较大,强度难以降低。
另外,自不必说,本发明不限于上述的实施方式,只要属于本发明的技术范围,则可利用各种方式来实施。
实施例
下面,将具体制造蜂窝过滤器10的例子作为实验例进行说明。
[实验例1]
首先,将6720重量份的作为粗粒碳化硅的α型碳化硅粉末(平均粒径22μm)、2880重量份的作为微粒碳化硅的α型碳化硅粉末(平均粒径0.5μm)、980重量份的作为成孔剂的丙烯酸树脂颗粒(平均粒径20μm)以及2970重量份的水混合,还添加1050重量份的作为有机粘合剂的甲基纤维素、500重量份的作为增塑剂的甘油、以及230重量份的润滑剂(商品名ユニル一ブ(UNILUBE);日本油脂社制),进行捏合,得到坯土。将该实验例1的蜂窝过滤器10的原料、各原料的平均粒径、添加量的各数值等归纳示于表1。并且,该表1中还归纳示出了后述的实验例2~34相关的内容。接着,利用挤出成型机对该坯土进行挤出成型,形成有沿长度方向并排的多个贯通孔12的棱柱状,得到没有形成封孔部14的蜂窝过滤器10的形状的粗成型体。接着,利用微波干燥机和热风干燥机对得到的粗成型体干燥,对于多个贯通孔12,利用封孔部14以一方的端面被封孔而另一方的端面开口的贯通孔12与一方的端面开口而另一方的端面被封孔的贯通孔12交错并排的方式进行封孔,所述封孔部14使用与上述坯土组成相同的糊。然后,进一步进行干燥,在400℃下脱脂3小时。在常压的氩气氛下以2200℃将该成型体烧制3小时,由此,制作了由碳化硅构成的蜂窝结构体(参照图1),其为34.3mm×34.3mm×150mm、贯通孔为46.5个/cm2(300cpsi)、壁部15的厚度为0.43mm、与贯通孔12垂直相交的面的开口率为50%。
表1
样品 | 粗粒SiC径量 | 微粒SiC径量 | 丙烯酸树脂颗粒径量 | 甲基纤维素 | 水 | 增塑剂润滑剂 | ||||
μm | 重量份 | μm | 重量份 | μm | 重量份 | 重量份 | 重量份 | 重量份 | 重量份 | |
实验例1~5实验例6~10实验例11~15实验例16~20实验例21~25实验例26~30实验例31,32实验例33,34 | 2211112240223050 | 67206720672045504550455045506720 | 0.50.50.50.50.50.50.50.5 | 28802880288019502880288019502880 | 206040/604040/6020/406040 | 980980490/4901060530/530530/5301060980 | 1050105010505505505505501050 | 29702970297015001500150015002970 | 500500500330330330330500 | 230230230150150150150230 |
接着,在该蜂窝结构体上担载作为催化剂的铂。首先,在200重量份的水中添加100重量份的活性氧化铝粉末(平均粒径2μm),加入20重量份的硝酸,调制涂覆用浆料。将蜂窝结构体浸渍于该浆料中,提起之后,去除多余的浆料,在250℃干燥15分钟。氧化铝的担载量达到蜂窝过滤器10的每单位体积上的重量为80g/L。接着,调制0.25mol/L的硝酸铂溶液,使蜂窝结构体吸收该硝酸铂溶液,使得铂的担载量达到蜂窝过滤器10的每单位体积上铂的重量为3.0g/L,在600℃下烧制1小时。这样,得到图1所示的蜂窝过滤器10。
将该实验例1的蜂窝过滤器10的蜂窝过滤器10的开口率、蜂窝过滤器10的开口率C、壁部15的壁厚和孔密度的各数值等归纳示于表2。该表2还归纳示出了后述的实验例2~34相关的内容。并且,该表2还归纳示出了后述的评价结果、即气孔径为10μm以下的气孔的容积相对于全部气孔容积的比例A、气孔径为30μm以上的气孔的容积相对于全部气孔容积的比例B以及A/B值。
表2
样品 | 10μm以下的容积比例A(%) | 30μm以上的容积比例B(%) | A/B值 | 开口率C(%) | 壁厚(mm) | 孔密度 | |
(cpsi) | (个/cm2) | ||||||
实验例1实验例2实验例3实验例4实验例5 | 0.50.50.50.50.5 | 17.117.117.117.117.1 | 0.030.030.030.030.03 | 50.052.958.060.160.4 | 0.430.400.350.330.40 | 300300300300200 | 46.546.546.546.531.0 |
实验例6实验例7实验例8实验例9实验例10 | 8.28.28.28.28.2 | 16.316.316.316.316.3 | 0.500.500.500.500.50 | 52.954.858.060.463.3 | 0.400.330.350.400.30 | 300400300200300 | 46.562.046.531.046.5 |
实验例11实验例12实验例13实验例14实验例15 | 16.616.616.616.616.6 | 19.919.919.919.919.9 | 0.830.830.830.830.83 | 52.954.960.161.263.3 | 0.400.380.330.350.30 | 300300300250300 | 46.546.546.538.846.5 |
实验例16实验例17实验例18实验例19实验例20 | 16.016.016.016.016.0 | 10.810.810.810.810.8 | 1.481.481.481.481.48 | 54.956.460.163.364.5 | 0.380.400.330.300.25 | 300250300300400 | 46.538.846.546.562.0 |
实验例21实验例22实验例23实验例24实验例25 | 19.919.919.919.919.9 | 10.910.910.910.910.9 | 1.831.831.831.831.83 | 56.458.060.464.565.5 | 0.400.350.400.250.28 | 250300200400300 | 38.846.531.062..046.5 |
实验例26实验例27实验例28实验例29实验例30 | 16.116.116.116.116.1 | 7.17.17.17.17.1 | 2.272.272.272.272.27 | 58.058.363.365.568.8 | 0.350.300.300.280.25 | 300400300300300 | 46.562.046.546.546.5 |
实验例31实验例32 | 21.021.0 | 10.010.0 | 2.102.10 | 60.463.3 | 0.400.30 | 200300 | 31.046.5 |
实验例33实验例34 | 9.49.4 | 22.622.6 | 0.420.42 | 56.258.0 | 0.450.35 | 200300 | 31.046.5 |
[实验例2~34]
按照表1所示的添加量来混合原料,设计成表2所示的开口率C、壁厚和孔密度,除此之外,采用与实验例1相同的方式,制作实验例2~34的蜂窝过滤器10。
[气孔径/气孔率测定]
进行实验例1~34的气孔径/气孔率测定。作为测定机使用(株)岛津制作所制的自动孔隙率测定仪AutoPore III9405,根据JIS-R1655,利用水银压入法来进行该测定。具体讲,将蜂窝过滤器10的不包含封孔部14的部分切割成1边为0.8cm左右的立方体,利用离子交换水进行超声波清洗,干燥之后,使用上述测定机,在0.1μm~360μm的测定范围内进行测定。在100μm~360μm的范围内,以每0.1psia的压力进行测定,在0.1μm~100μm的范围内,以每0.25psia的压力进行测定。另外,在该测定、压力损失测定和PM的捕获效率测定中,使用担载了作为涂覆层的催化剂载体(氧化铝)和催化剂(铂)之后的蜂窝过滤器10进行测定。
[压力损失测定]
进行实验例1~34的蜂窝过滤器10的压力损失测定。图5是压力损失测定装置40的说明图。该压力损失测定装置40是如下的装置:卷绕了氧化铝垫43的蜂窝过滤器10固定在金属套管44内,然后配置在送风机41的排气管42上,并且在送风机41的排气管42上安装有可检测蜂窝过滤器10的前后压力的压力计48。压力损失的测定条件如下:使送风机41运转,使得废气的流通量达到750m3/h,测定运转开始起5分钟后的压差。
[PM的捕获效率测定]
进行实验例1~34的废气中含有的PM的捕获效率测定。图6是废气净化测定装置60的说明图。该废气净化测定装置60构成为扫描型电移动微粒分析装置(Scanning Mobility Particle Sizer,SMPS),其包括:2L的共轨式柴油发动机61;排气管62,其用于流通来自发动机61的废气;金属套管64,其与排气管62连接,用于固定卷绕了氧化铝垫63的蜂窝过滤器10;取样器65,其对流通蜂窝过滤器10前的废气进行取样;取样器66,其对流通蜂窝过滤器10后的废气进行取样;稀释器67,其将利用取样器65、66取样的废气进行稀释;以及PM计数器68(TSI社制凝集粒子计数器3022A-S),其测定该稀释的废气中含有的PM量。接着,说明测定步骤。使发动机61以发动机旋转数为2000rpm、转矩为47Nm的方式运转,使来自发动机61的废气在蜂窝过滤器10内流通。此时,使用PM计数器68,根据PM颗粒数量来掌握通过蜂窝过滤器10之前的PM量PO和通过蜂窝过滤器10之后的PM量Pi。然后,使用下述式(4),求出废气中含有的PM的捕获效率。
捕获效率(%)=(P0-Pi)/P0×100;式(4)
[实验结果]
表3中归纳了实施例1~34的实验结果即A/B值、根据A/B值利用式(1)求出的开口率C的下限值Cmin和上限值Cmax、蜂窝过滤器10的开口率C、平均气孔径、气孔率、压力损失以及PM捕获效率,图7是针对实施例1~30(比例A为20%以下,比例B为20%以下的样品),将横轴设为A/B值,纵轴设为开口率C来描绘的A/B值和开口率C之间关系的图。另外,在图7中,将上述的式(1)范围内的实施例描绘成○,将式(1)的范围外的实施例描绘成△,将各实施例的号码标在各点上。由表3可知,比例A大于20%时(实验例31、32),压力损失增大,比例B大于20%时(实验例33、34),PM捕获效率降低。接着,由表3和图7可知,实验例2~4、7~9、12~14、17~19、22~24、27~29的样品,即进入图4的优选范围(满足式(1)的范围)的样品中,压力损失为13kPa以下,且PM捕获效率为80%以上,可降低压力损失并充分捕获PM。而且知道了开口率C为54%以上时,压力损失较小。并且,实验例3~4、8~9、13~14、18~19、23~24、28~29的样品,即在满足2.5×A/B+55.5≤C的样品中,压力损失显示出了更小的值。并且,在实验例2、7~8、12~13、17~18、22~23、27~28的样品,即满足C≤2.5×A/B+58.0的样品中,PM的捕获效率显示出了更大的值。尤其,在2.5×A/B+55.5≤C≤2.5×A/B+58.0的范围的实验例8、13、18、23、28中,压力损失和PM捕获效率之间的平衡最佳。
表3
样品 | A/B值 | 开口率1)下限值 | 开口率2)上限值 | 开口平C | 平均气孔径 | 气孔率 | 压力损失 | 粒状物质捕获率 |
Cmin | Cmax | (%) | (μm) | (%) | (kPa) | (%) | ||
实验例1实验例2实验例3实验例4实验例5 | 0.030.030.030.030.03 | 52.652.652.652.652.6 | 60.360.360.360.360.3 | 50.052.958.060.160.4 | 20.820.820.B20.820.8 | 58.158.158.158.158.1 | 13.612.812.412.212.2 | 9290848076 |
实验例6实验例7实验例8实验例9实验例10 | 0.500.500.500.500.50 | 53.853.853.853.853.8 | 61.561.561.561.561.5 | 52.954.858.060.463.3 | 20.020.020.020.020.0 | 60.060.060.060.060.0 | 13.712.812.512.312.1 | 9089868273 |
实验例11实验例12实验例13实验例14实验例15 | 0.830.830.830.830.83 | 54.654.654.654.654.6 | 62.362.362.362.362.3 | 52.954.960.161.263.3 | 19.819.819.819.819.8 | 57.657.657.657.657.6 | 13.812.912.612.412.2 | 9390868476 |
实验例16实验例17实验例18实验例19实验例20 | 1.481.481.481.481.48 | 56.256.256.256.256.2 | 63.963.963.963.963.9 | 54.956.460.163.364.5 | 18.118.118.118.118.1 | 58.758.758.758.758.7 | 13.413.012.412.312.2 | 9090868278 |
实验例21实验例22实验例23实验例24实验例25 | 1.831.831.831.831.83 | 57.157.157.157.157.1 | 64.864.864.864.864.8 | 56.458.060.464.565.5 | 17.917.917.917.917.9 | 57.957.957.957.957.9 | 13.512.812.612.412.4 | 9292888277 |
实验例26实验例27实验例28实验例29实验例30 | 2.272.272.272.272.27 | 58.258.258.258.258.2 | 65.965.965.965.965.9 | 58.058.363.365.568.8 | 17.617.617.617.617.6 | 57.157.157.157.157.1 | 13.412.812.412.312.1 | 9290888574 |
实验例31实验例32 | 2.102.10 | 57.857.8 | 65.565.5 | 60.463.3 | 19.619.6 | 58.458.4 | 14.113.6 | 9086 |
实验例33实验例34 | 0.420.42 | 53.553.5 | 61.261.2 | 56.258.0 | 21.721.7 | 58.958.9 | 12.412.1 | 7269 |
1)根据Cmin=2.5×A/B+52.5算出
2)根据Cmax=2.5×A/B+60.2算出
[过滤器集合体]
制作多个上述的实验例1~34的蜂窝过滤器10,将它们作为蜂窝单元11,在蜂窝单元11的外表面13上涂布密封材料,将多个蜂窝单元11接合,在120℃对密封材料进行干燥、固化,形成密封材料层26。密封材料使用各组分如下的混合物:30重量%的氧化铝纤维(纤维长20μm)、21重量%的碳化硅颗粒(平均粒径0.6μm)、15重量%的氧化硅溶胶(溶胶中的氧化硅含量为30重量%)、5.6重量%的羧甲基纤维素、28.4重量%的水。接着,使用金刚石刀具将该接合的过滤器切削加工成圆柱状,使用涂覆材料对没有贯通孔12开口的外周面进行涂布,在120℃进行干燥、固化,形成涂覆材料层27。涂覆材料使用各组分为如下的混合物:23.3重量%的氧化硅-氧化铝纤维(纤维长5μm~100μm)、30.2重量%的碳化硅颗粒(平均粒径0.3μm)、7重量%的氧化硅溶胶(溶胶中的氧化硅含量为30重量%)、0.5重量%的羧甲基纤维素、39重量%的水。接着,与上述蜂窝过滤器10同样地涂布催化剂载体之后,担载催化剂,得到图3所示的蜂窝过滤器20。蜂窝单元11的总截面积相对于得到的蜂窝过滤器20的截面积所占的比例(单元面积比例)为93.5%。
本发明是以2004年12月28日申请的日本国专利申请2004-382132号为要求优先权的基础,编入其内容的全部。
产业上的可利用性
本发明可利用于装配了内燃机的动力机和车辆等相关的产业,可利用于例如汽车产业、摩托车产业等。
Claims (10)
1.一种过滤器,该过滤器具有多个贯通孔,其特征在于,
当将所述贯通孔彼此之间的壁部上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A%,将该壁部上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B%,将与所述贯通孔垂直相交的面的开口率设为C%时,该过滤器满足2.5×A/B+52.5≤C≤2.5×A/B+60.2,其中A≤20,0<B≤20。
2.一种过滤器,该过滤器具有多个贯通孔,其特征在于,
在所述贯通孔彼此之间的壁部上担载有催化剂,
当将所述壁部上的气孔径为10μm以下的气孔相对于全部气孔容积所占的比例设为A%,将该壁部上的气孔径为30μm以上的气孔相对于全部气孔容积所占的比例设为B%,将与所述贯通孔垂直相交的面的开口率设为C%时,该过滤器满足2.5×A/B+52.5≤C≤2.5×A/B+60.2,其中A≤20,0<B≤20。
3.根据权利要求1或2所述的过滤器,其特征在于,该过滤器还满足2.5×A/B+55.5≤C。
4.根据权利要求1~3的任意一项所述的过滤器,其特征在于,该过滤器还满足C≤2.5×A/B+58.0。
5.根据权利要求1~4的任意一项所述的过滤器,其特征在于,所述开口率为58%以上。
6.根据权利要求1~5的任意一项所述的过滤器,其特征在于,所述开口率为75%以下。
7.根据权利要求1~6的任意一项所述的过滤器,其特征在于,所述贯通孔彼此之间的壁厚为0.15mm~0.40mm。
8.根据权利要求1~7的任意一项所述的过滤器,其特征在于,该过滤器的孔密度为31个/cm2~78个/cm2。
9.根据权利要求1~8的任意一项所述的过滤器,其特征在于,该过滤器以碳化硅、氮化硅以及堇青石之中的任意一种作为主成分。
10.一种过滤器集合体,其特征在于,该过滤器集合体中,2个以上的权利要求1~9的任意一项所述的过滤器以没有所述贯通孔开口的外表面通过密封材料层接合在一起。
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JPWO2006070504A1 (ja) | 2008-06-12 |
US20060254231A1 (en) | 2006-11-16 |
JP4874812B2 (ja) | 2012-02-15 |
EP1707251A1 (en) | 2006-10-04 |
US7341614B2 (en) | 2008-03-11 |
EP1707251A4 (en) | 2011-01-19 |
CN100450577C (zh) | 2009-01-14 |
EP1707251B1 (en) | 2012-10-10 |
KR20070085073A (ko) | 2007-08-27 |
KR100820619B1 (ko) | 2008-04-08 |
WO2006070504A1 (ja) | 2006-07-06 |
PL1707251T3 (pl) | 2013-03-29 |
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