CN101454129A - 陶瓷蜂窝过滤器的制造方法 - Google Patents
陶瓷蜂窝过滤器的制造方法 Download PDFInfo
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- CN101454129A CN101454129A CNA2007800189261A CN200780018926A CN101454129A CN 101454129 A CN101454129 A CN 101454129A CN A2007800189261 A CNA2007800189261 A CN A2007800189261A CN 200780018926 A CN200780018926 A CN 200780018926A CN 101454129 A CN101454129 A CN 101454129A
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- mixing
- base soil
- honeycomb filter
- ceramic honeycomb
- carry out
- Prior art date
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Images
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Abstract
本发明提供一种陶瓷蜂窝过滤器的制造方法,通过对含有陶瓷原料、成形助剂及造孔材料的原料混合物进行混炼,制作蜂窝状挤压成形体用的坯土,其特征在于,通过加压式捏合机以0.12~0.5MPa的加压力进行混炼。
Description
技术领域
本发明提供一种废气气体净化用陶瓷蜂窝过滤器的制造方法,特别是涉及形成挤压成形体的陶瓷原料的混炼方法。
背景技术
在柴油发动机的废气中含有以碳(煤等)及高沸点碳化氢为主要成分的微粒子(particulate matter),将其排放入大气时,可能会给人及环境带来恶劣影响。因此,在柴油的排气管的中途,一直以来安装有用于除去微粒子并净化废气气体的陶瓷蜂窝过滤器(以下称为“蜂窝过滤器”)。如图2所示,蜂窝过滤器20由形成多个通路5、6的多孔质隔壁7和外周壁8构成的陶瓷蜂窝构造体21、将通路5、6的两端面9、10以棋盘格规格相互密封的密封部11a、11b构成。
在上述蜂窝构造体21的制造中,多使用在陶瓷原料、成形助剂、用于制作隔壁内部的气孔的造孔材料等混合物中加水进行混炼,制作蜂窝状挤压成形体用坯土(以下,略称为坯土),将其挤压成形后,进行烧结而作成蜂窝构造体的方法。作为上述那样的过滤器使用的蜂窝构造体,为了同时实现对废气气体中微粒子状物质的捕集效率的提高和压力损失的降低,需要控制气孔径和气孔率。气孔径及气孔率的控制目前为止是通过调节石炭粉、小麦粉等造孔材料的添加量来进行。近年来,为了以更低的热膨胀得到气孔率高的蜂窝构造体,将例如特开2003—38919号所记载的微胶囊(内包气体的中空树脂)作为造孔材料使用。
在陶瓷原料、造孔材料等混合物中加水进行混炼的工序中,尤为重要是对坯土进行均质混炼,同时将坯土中的空气尽可能的除去。坯土未均质混炼,或坯土中的空气未充分除去时,蜂窝构造体产生缺陷。
将坯土均质混炼时,作为减少坯土中的残存空气的技术,特开2005—271395号中开示有:由在出口配置了设有用于将坯土细分化的多个的通路的细分盘的第一圆筒、和经由上述细分盘的多个通路使坯土流入内部而将坯土进一步混炼且真空脱气的第二圆筒构成的螺旋桨式的真空土炼机。然而,由于内包有气体的中空树脂即微胶囊对剪断力比较弱,故在使用记载于特开2005—271395号螺旋桨式土炼机的情况下,会产生在混炼过程中作用的过度的剪断力破坏微胶囊,使蜂窝构造体的气孔率减小这样的问题。其中,在微胶囊的外皮(外壳)的厚度为0.1~2μm这样薄的情况下,微胶囊很容易被破坏,特别是外壳的厚度为0.1~0.8μm这样的情况下尤为显著,存在蜂窝构造体的气孔率明显小这样的问题。为了得到希望的气孔率而添加大量的微胶囊制作坯土时,坯土的粘度变小,造成挤压成形后的蜂窝成形体的保型性恶化,且蜂窝构造体的尺寸精度恶化。因此,难以制造通路垂直方向剖面的直径为180mm以上这样的大型且气孔率大的蜂窝制造体。降低混炼速度并以低的剪断力进行混炼时,虽然微胶囊的破坏减少,得到的蜂窝构造体的气孔率增大,但不会得到混炼充分且均一的坯土。在这样的不均一的坯土中存在流动性不同的微少部分,会产生在挤压成形后的蜂窝成形体的隔壁上产生切断或弯曲这样的不良。从这样的不均一的成形体得到的陶瓷蜂窝过滤器会产生由于隔壁的切断引起的微粒子的捕集率降低、及由于隔壁的弯曲引起的压力损失上升。
特开2006—264237号开示有将含有陶瓷材料的成形原料进行混合·混炼后,通过土炼机挤压得到的坯土按希望的长度切断,由活塞式的挤压成形机形成蜂窝成形体的方法。在使用特开2006—264237号记载的土炼机的情况下,也会产生由于在混炼中施加的过度的剪断力而使微胶囊破坏,使得蜂窝构造体的气孔率减小这样的问题。
另一方面,在使用通过两个转子的旋转进行混炼的捏合机的方法的情况下,由于容易卷进坯土中,故容易在蜂窝构造体上产生缺陷。因此,捏合机进行的坯土的混炼不太可行。
发明内容
因此,本发明的目的为提供一种以混合效率高,通过不过度剪断的混炼方法,防止微胶囊破坏的同时气孔率高的不存在切断及弯曲不良及缺陷的蜂窝构造体。
鉴于所述目的锐意研究的结果是,本发明者等发现,通过浪涌加压式捏合机进行混炼,得到气孔率高,没有缺陷的陶瓷蜂窝过滤器,想到本发明。
即,本发明提供一种制造陶瓷蜂窝过滤器的方法,通过对含有陶瓷原料、成形助剂及造孔材料的原料混合物进行混炼,制作蜂窝状挤压成形体用的坯土,其特征在于,通过加压式捏合机以0.12~0.5MPa的加压力进行混炼。
混炼后的所述坯土的类型C肖氏硬度(以JIS K7312为基准)优选为16~23。
优选为在减压环境下进行混炼。所述减压环境优选为真空度以标准压计为2×10-2MPa以上。
混炼时的所述坯土的温度优选为15~35℃。
混合后的坯土优选为使用活塞式的挤压成形机挤压成形为蜂窝的形状。
本发明另一方面提供一种制造陶瓷蜂窝过滤器的方法,通过对含有陶瓷原料、成形助剂及造孔材料的原料混合物进行混炼,制作蜂窝状挤压成形体用的坯土,其特征在于,通过加压式捏合机以0.12~0.5MPa的加压力进行混炼后,使用直接活塞式的挤压成形机挤压成形为蜂窝状。
本发明的方法由于通过降低对微胶囊作用的过度的剪切力的方法进行混炼,故可以防止微胶囊的破坏,可以得到具有气孔率为50~70%且60~70%大的蜂窝构造体。特别是适合作为得到通路垂直方向剖面的直径为180mm以上的大型且气孔率大的构造体的方法。另外,由于降低了坯土中的残留空气,故可以防止断裂及弯曲不良的发生。
附图说明
图1(a)是表示本发明中使用的加压式捏合机剖面图;
图1(b)是表示将本发明中使用的加压式捏合机的加压盖卸下后的状态的上面图;
图2是表示陶瓷蜂窝之一例的模式剖面图;
图3是表示活塞式挤压成形机之一例的剖面图。
具体实施方式
(1)加压式捏合机
本发明者进行锐意讨论的结果发现,混炼工序中的微胶囊的破坏引起的蜂窝构造体的气孔率的低下的问题、及由坯土中的残存气体及混炼不足引起的蜂窝构造体的断裂及弯曲不良的问题,可以通过将含有陶瓷原料、成形助剂及造孔材料的原料通过加压式捏合机混炼得以解决。加压式捏合机如图1(a)所示,具有通过加压盖3对混炼槽1内的原料(未图示)进行加压,同时通过转子2进行混炼的构造。在转子2上,如图1(b)所示,交互配置有二片叶片2a,两个转子2以叶片相互不碰撞的方式进行配置。两个转子可以同步转动也可以独立转动。混炼槽1内的原料通过加压盖3的荷重、活塞轴4的荷重、及通过活塞轴4对加压盖3挤压的力P进行加压。由于加压下的混炼与非加压式的捏合机相比混炼效率良好,故可以缩短混炼时间。
存在上述那样的捏合机的混炼容易在坯土中卷进空气这样的问题,但发明者发现通过提高加压式捏合机的压力可以显著减少坯土中的残存空气。加压力越高效果越大,若为0.12MPa以上,则可以将蜂窝构造体的缺陷降低到实用上没有问题的程度。在加压力低于0.12MPa的情况下,由于空气残存并且由转子向加压盖方向卷起的坯土停滞于加压盖的正下方,故混炼不足,因此,造成成形时挤压速度不均一。因此,得到的蜂窝构造体发生断裂及弯曲不良。
另一方面,加压力过高时,过度的剪断力增加而破坏微胶囊。特别是在加压力高于0.5MPa的情况下尤为显著。通过将加压力设为0.5MPa以下,与使用螺旋桨式土炼机的情况相比,可防止微胶囊的破坏,可以得到气孔率大的蜂窝构造体。特别是在陶瓷原料粉末中含有粉碎非晶体物的粒子(非晶体硅石等)的情况下,由于以非晶体粒子的棱角形状容易破坏微胶囊,故优选为进一步降低加压力以不使微胶囊遭到破坏。在加压力高于0.5MPa的情况下,加压盖妨碍转子引起的坯土的卷起,有时产生混炼不足。因此,得到的蜂窝构造体发生断裂及弯曲不良。特别是陶瓷原料的平均粒径为0.1~30μm的情况及混炼相对于原料粉末100份添加了10~30份的水分的状态的坯土时,容易发生断裂及弯曲不良。
因此,加压式捏合机的加压力为0.12~0.5MPa,优选为0.15~0.4MPa。另外,上述加压力为(活塞轴4对加压盖3的推力P+加压盖3的荷重+活塞轴4的荷重)除以加压盖3的原料接触面面积A的值。
加压式捏合机如上所述,具有在短时间内可以将坯土均一混炼的优点,同时,通过适当设定加压力可以降低卷入混炼中的空气,但为了进一步除去坯土中的空气,优选在减压环境下进行混炼。通过将混炼时的真空度设为在标准压下为2×10-2MPa以上,可以在更短时间内除去坯土中的空气。因此,如特开2005—271395号记载的那样,即使没有将混炼后的坯土挤压为面状,除去坯土中的空气的工序,仅靠在混合混炼机的混炼,也可以防止蜂窝成形体的隔壁上断裂等不良的产生。真空度为标准压(与大气压的压差)所示的值,值越大真空度越高。在本发明中,混炼时的真空度更优选为4×10-2MPa以上,进一步优选为5×10-2MPa以上。在真空度为极端高时,混炼中的坯土的水分蒸发,特别是在含水量少的坯土及温度高的坯土的情况下,混炼后的坯土的硬度变高。因此,真空度优选为8.5×10-2MPa以下。
优选为只通过上述加压式捏合机的混炼结束混炼工序。另外,在加压式捏合机的混炼工序之后,在将坯土挤压成形为蜂窝状成形体的成形工序中,如图3所示,优选使用活塞式的挤压成形机30。图3中,坯土11通过由活塞12挤压,得到蜂窝成形体13。通过使用活塞式的挤压成形机30,可以将作用于坯土11中的微胶囊的剪断降至最小限,可以防止微胶囊的破坏。活塞式的挤压成形优选在加压式捏合机的混炼之后进行。土炼机的混炼及螺旋桨式的挤压成形机的使用除招致微胶囊的破坏且蜂窝构造体的气孔率低下之外,由于螺旋桨的轴附近和外周部的混炼程度也同,或坯土的温度局部升高,从而坯土的粘性也会不均一。
(2)坯土
为了进一步降低对混炼时的微胶囊施加的剪断力,坯土优选为柔软的坯土。通过降低坯土的硬度,可防止微胶囊的破坏,进一步增大蜂窝构造体的气孔率。混炼后的坯土的类型C肖氏硬度(以JIS K7312为基准)(以下只称为肖氏硬度)优选为23以下,更优选为22以下。另一方面,坯土的硬度过低时,挤压成形后的成形体由于自重而发生形变。因此,混炼后的坯土的肖氏硬度优选为16以上,更优选为18以上。肖氏硬度可以通过相对于陶瓷原料的水的添加量进行调整。
混炼时的坯土的温度优选为15~35℃。坯土的温度低时粘度低,挤压成形后的成形体容易由于自重而容易变形。通过将混炼中的坯土的温度设为15℃以上,即使挤压成形时不加热,由于坯土的粘度高,故也可以减小成形体的变形量。另一方面,在坯土中含有作为黏合剂的甲基纤维素的情况下,坯土的温度过高时,粘度显著升高,容易在蜂窝状成形体的隔壁上产生断裂及弯曲。由于一旦粘度较高时,即使温度降低后粘度也不容易下降,因此,混炼中的坯土的温度优选为保持在35℃以下。坯土的温度的更优选为20~30℃。由于混炼中的坯土的温度随着通常时间上升,故只要混炼结束时的温度在上述的范围内即可。混炼结束时的温度在混炼结束后的3分钟内在土块内部插入温度计进行测定。
(3)陶瓷原料
陶瓷原料没有特别限定,优选含有例如:堇青石、氧化铝、模来石、氮化硅、塞隆、碳化硅、钛酸铝、氮化铝及LAS等中的至少一种。其中,以堇青石为主结晶的陶瓷蜂窝构造体热膨胀系数低,耐热冲击性良好,故优选之。
(4)造孔材料
造孔材料优选被内部包含气体的树脂制的外壳包围的微胶囊。通过使用这样的造孔材料,可以显著发挥本发明的效果。微胶囊更优选为发泡完成的发泡树脂,外壳的厚度优选为0.1~0.8μm。树脂没有特别限定,优选为丙烯系、异丁烯酸脂系、羟酸系等。微胶囊的添加量根据作为目标的蜂窝构造体的气孔率等而不同,为了得到气孔率大的蜂窝构造体,相对于陶瓷原料优选为4~13质量%,更优选为5~10质量%。另外,微胶囊中还可以混合其他的造孔材料(以石墨等碳为主要成分的粉末、小麦粉、玉米粉等淀粉粉末及聚对苯二甲酸乙酯、聚甲基丙烯酸甲酯等树脂粉末)的一种或两种以上。
接下来,通过实施例具体地说明本发明,但本发明不限于这些实施例。
实施例1
在图1所示的加压式混合的混炼槽1内,将高岭土、滑石、二氧化硅、氧化铝、氧化铝的粉末以达到50质量%的SiO2、35质量%的Al2O3、及15质量%的MgO的组成配合,作成堇青石生成原料粉末。向其中投入作为成形助剂的甲基纤维素及羟丙基甲基纤维素、润滑材料、作为造孔材料的发泡树脂以及水,加压力为0.5MPa下不对混炼层1内减压而混炼50分钟,制作陶瓷坯土。对混炼结束时的坯土的温度及肖氏硬度进行测定。结果如表1所示。
将得到的坯土用直接活塞式挤压成形机进行挤压成形,得到直径180mm、长度180mm、隔壁的厚度0.3mm、隔壁距离1.5mm的蜂窝生形体。其次,将该蜂窝成形体以其通路方向为上下方向的方式置于定盘中干燥5小时,对干燥前后的全长进行测定,从其差求其收缩量,通过以下的基准进行评价。结果如图表1所示。
判断为几乎不收缩的装置(收缩量不足3%)…◎
有收缩但实用上没有问题的装置(收缩量3~4%)…○
判断为因收缩而在实用上产生问题的装置(收缩量超过4%)…×
将干燥后的蜂窝成形体在1400℃下烧结4小时,制造蜂窝构造体。对该蜂窝构造体的气孔率浪涌水银压入法进行测定,断裂和弯曲不良以以下的基准通过目视评价。结果如图1所示。
存在断裂或弯曲不良的构造体…×
存在断裂或弯曲不良但实用上没有的构造体…○
存在断裂或弯曲不良不能确认的构造体…◎
实施例2~5
除将加压力如表1所示那样变更以外,与实施例1同样地进行混炼,制作坯土。这些实施例的加压力及坯土温度如表1所示。使用这些的坯土与实施例1同样地进行成形体的制作、收缩量的测定、蜂窝成形体的烧结、气孔率的测定、断裂和弯曲不良的评价。结果如表1所示。
实施例6~10
除将坯土温度及/或肖氏硬度如表1所示那样变更以外,与实施例3同样地进行混炼,坯土制作。这些实施例的加压力坯土温度及肖氏硬度如表1所示。使用这些的坯土与实施例1相同地进行成形体的制作、收缩量的测定、蜂窝成形体的烧成、气孔率的测定、断裂和弯曲不良的评价。结果如表1所示。
实施例11~16
除将坯土温度、肖氏硬度及/或混炼槽1内的真空度如表1所示那样变更以外,与实施例3同样地进行混炼,坯土制作。这些实施例的加压力坯土温度及肖氏硬度如表1所示。使用这些坯土与实施例1相同地进行成形体的制作、收缩量的测定、蜂窝成形体的烧成、气孔率的测定、断裂和弯曲不良的评价。结果如表1所示。
比较例1~6
除将加压力、真空度、混炼后的坯土的温度及肖氏硬度如表1所示那样变更以外,与实施例1同样地进行混炼,制作比较例1~4的坯土。
使用螺旋桨式混炼机不进行减压地进行混炼,其后,使用螺旋桨式挤压成形机进行成形,除此之外,与实施例1同样地进行混炼,制作比较例5的坯土。
除将混炼时间变更为70分钟外,与实施例1同样地进行混炼,制作比较例6的坯土。
比较例1~6的混炼时的加压力、真空度、以及得到的坯土的温度及肖氏硬度如表1所示,使用这些坯土与实施例1同样地进行成形体的制作、收缩量的测定、蜂窝成形体的烧成、气孔率的测定、断裂和弯曲不良的评价。结果如表1所示。
表1
注*:真空度表示标准压(与大气压的压差)
表1(续表)
通过实施例1~16及比较例1~6的结果,以0.12~0.5MPa的加压力进行混炼的实施例1~16的情况下,气孔率高达61~64%,断裂或弯曲不良不能确认、或为未达到实用上的问题的水平。然而,以不足0.12MPa的加压力混炼的比较例1及2的情况下,可以发现坯土中空气的残存和混炼不足引起的断裂或弯曲不良,得知在50分钟之内混炼不能完成。以大于0.5MPa的加压力混炼的比较例3及4的情况下,得知烧结后的蜂窝构造体的气孔率缩小至54~57%,混炼中发泡完成的发泡树脂被破坏,加压力特别大到1.0MPa的比较例4的情况下,确认断裂及弯曲不良。在使用螺旋桨式混炼机的比较例4的情况下,得知烧结后的蜂窝构造体的气孔率缩小至52%,混炼中的发泡树脂被破坏。另外,由于混炼中不进行减压,故确认了断裂或弯曲不良。不施加加压力地进行混炼的比较例6中,发现坯土中的空气的残存和混炼不足引起断裂和弯曲不良,得知尽管将混炼时间延长1.4倍,但混炼仍不能完成。
相对于肖氏硬度为24的实施例3,得知肖氏硬度为16~23的实施例6~10中气孔率高,发泡树脂的成品率进一步提高。混炼时以标准压2×10-2MPa以上的真空度进行混合槽1的减压,在将坯土温度调制为30℃以下,肖氏硬度调制为22以下的实施例12~15的情况下,对实施例1~5不能完全确认断裂或弯曲不良。特别是坯土温度在20℃以上,肖氏硬度为18以上的实施例12~14中几乎不引起收缩,特别良好。
Claims (8)
1、一种陶瓷蜂窝过滤器的制造方法,对含有陶瓷原料、成形助剂及造孔材料的原料混合物进行混炼,制作蜂窝状挤压成形体用的坯土,其特征在于,通过加压式捏合机以0.12~0.5MPa的加压力进行混炼。
2、如权利要求1所述的陶瓷蜂窝过滤器的制造方法,其特征在于,混炼后的所述坯土的类型C肖氏硬度(以JIS K7312为基准)为16~23。
3、如权利要求1或2所述的陶瓷蜂窝过滤器的制造方法,其特征在于,在减压环境下进行混炼。
4、如权利要求3所述的陶瓷蜂窝过滤器的制造方法,其特征在于,在真空度以标准压计为2×10-2MPa以上的减压环境下进行混炼。
5、如权利要求1~4中任一项所述的陶瓷蜂窝过滤器的制造方法,其特征在于,混炼时的所述坯土的温度为15~35℃。
6、如权利要求1~5中任一项所述的陶瓷蜂窝过滤器的制造方法,其特征在于,具有将混炼后的坯土使用活塞式的挤压成形机挤压成形为蜂窝状的工序。
7、一种陶瓷蜂窝过滤器的制造方法,对含有陶瓷原料、成形助剂及造孔材料的原料混合物进行混炼,制作蜂窝状挤压成形体用的坯土,其特征在于,通过加压式捏合机以0.12~0.5MPa的加压力进行混炼后,使用直接活塞式的挤压成形机挤压成形为蜂窝状。
8、如权利要求7所述的陶瓷蜂窝过滤器的制造方法,其特征在于,在真空度以标准压计为2×10-2MPa以上的减压环境下进行混炼。
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