CN1609417A - 蜂巢状结构体的制造方法及蜂巢状结构体 - Google Patents

蜂巢状结构体的制造方法及蜂巢状结构体 Download PDF

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CN1609417A
CN1609417A CNA2004100782876A CN200410078287A CN1609417A CN 1609417 A CN1609417 A CN 1609417A CN A2004100782876 A CNA2004100782876 A CN A2004100782876A CN 200410078287 A CN200410078287 A CN 200410078287A CN 1609417 A CN1609417 A CN 1609417A
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honeycomb structure
particle diameter
raw materials
raw material
mean particle
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CN1324226C (zh
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野口康
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NGK Insulators Ltd
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Abstract

本发明涉及蜂巢状结构体的制造方法和蜂巢状结构体。所述蜂巢状结构体的制造方法使用在蜂巢状结构体制造过程中产生的来自蜂巢状结构体的初始原料的回收物再生的再生原料作为初始原料的一部分，该再生原料被粉碎至平均粒径为10～2000μm，且平均粒径为2800～100000μm的粒子为0～10重量％蜂巢状结构体蜂巢状结构体。本发明的蜂巢状结构体的制造方法和蜂巢状结构体，在使用在蜂巢状结构体的制造过程中产生的来自蜂巢状结构体的初始原料的回收物制造蜂巢状结构体时，具有与使用原来的初始原料的场合相同程度的低热膨胀性和气孔率，同时可以提高成品率和大幅度降低费用。

Description

蜂巢状结构体的制造方法及蜂巢状结构体
技术领域
本发明涉及蜂巢状结构体的制造方法及蜂巢状结构体。
背景技术
作为捕集除去柴油机发动机排气那样的含尘流体中所含有的粒子状物质用的过滤器(柴油机颗粒过滤器)、或载附用于净化排气中的有害物质的催化剂成分(排气净化用)的催化剂载体，广泛使用由形成有若干个分别邻接的单元的复合体的单元隔壁(加强筋)、和位于该单元复合体的最外周的环绕保持最外周单元的蜂巢体外壁构成的多孔质的蜂巢状结构体，另外，作为其结构材料，使用着耐火性的碳化硅(SiC)和堇青石等，或者它们的复合材料等。
另外，正在进行采用在以往的柴油机颗粒过滤器上载附氧化催化剂、氧化和燃烧堆积的微粒从而连续再生的再生方式的柴油机颗粒过滤器(催化剂再生用柴油机颗粒过滤器)的开发。
但是，作为经济地制造上述蜂巢状结构体的方法，由在蜂巢状结构体的制造过程中产生的来自蜂巢状结构体的初始原料的回收物(例如从干燥工序移往烧成工序时，因某种原因遗漏的未煅烧的成形体或其碎片等未烧成的干燥物(SiC的场合下也包含烧成品))，可以调制(再生)初始原料组合物，并作为再生原料再次用于成形体的成形，在提高成品率和降低费用方面是令人满意的。
对于堇青石和陶瓷体的场合，因为要作为再生原料使用，要是粉碎作为回收物的未烧成的干燥物，使用其粉碎粉末制造的堇青石和陶瓷体，在多数场合与用原来的初始原料制造的堇青石和陶瓷体相比，热膨胀系数要大，耐热冲击性也下降，所以存在不能作为排气净化用蜂巢状催化剂载体使用的问题。
为了解决上述问题，分别提出了如下堇青石和陶瓷体及其制造方法的方案，例如，将作为回收物的未烧成的干燥物，经过在粗粉碎工序中破碎、粉碎和分级，作为调制(再生)的再生原料使用(参阅特许第1703709号公报)；从再生原料除去在未烧成的再生原料中所含的至少一部分粘合剂后，粉碎再生原料而制作成粉碎粉、在粉碎粉中加入水、粘合剂等，并且混炼，由此制作再生坯土，将再生坯土成形、烧成(参阅特开2000-302533号公报)；粉碎未烧成的再生原料、制成粉碎物，由此粉碎物除去直径小于1mm的粉碎物，向剩余的粉碎物中加入水，并且混炼，由此制成再生粘土，将再生粘土成形、烧成(参阅特开平8-119726号公报)。
但是，在特许第1703709号公报的方法中，将上述再生原料的粒度粉碎到小于10μm的场合，不仅粉碎效率差、花费费用，而且粉碎设备的磨损会变大，并有可能杂质的混入会增多。
在特开2000-302533号公报的方法中，因为对再生原料进行热处理等除去粘合剂，所以制造费用高；在特开平8-119726号公报的方法中，由于除去了小于等于1mm的再生原料，再生原料的收率差，再生原料也粗，所以混炼中的溶解不充分，蜂巢成形时可能发生堵塞等。
另外，在制造柴油机颗粒过滤器的场合，为了增大气孔率，需要使用粗的原料。要是使用平均粒径小于等于45μm的粒子超过20重量％、已粉碎的再生原料，会有得到的柴油机颗粒过滤器的平均气孔直径变小的问题。
进而，制造柴油机颗粒过滤器的场合，要是使用平均粒径大于等于2800μm的粒子超过10重量％、已粉碎的原料，在混炼、土炼工序中，再生原料就不能充分溶解，在成型时，堵塞喷嘴，得到的蜂巢状结构体中有发生单元缺陷的危险。
发明内容
本发明鉴于上述已有的技术问题而完成，其目的在于，在蜂巢状结构体的制造过程中，使用回收的未烧成的再生原料(SiC的场合烧成物也可以)制造蜂巢状结构体的时，提供具有和使用原来的初始原料的情况下同样程度的低热膨胀性和气孔率、同时可以提高成品率与大幅度地削减费用的蜂巢状结构体的制造方法和蜂巢状结构体。
即，通过本发明提供蜂巢状结构体的制造方法和蜂巢状结构体，所述蜂巢状结构体的制造方法使用在蜂巢状结构体制造过程中产生的来自蜂巢状结构体的初始原料的回收物再生的再生原料作为初始原料的一部分，其特征在于，该再生原料被粉碎至平均粒径为10～2000μm，且平均粒径为2800～100000μm的粒子为0～10重量％。
此时，在本发明中，优选上述再生原料被粉碎至平均粒径为100～1000μm，平均粒径为0.1～45μm的粒子为1～20重量％，并且粒径为1400～100000μm的粒子为0～10重量％。
另外，本发明中，上述回收物优选是未烧成的干燥物，蜂巢状结构体优选堇青石材质。
进而，本发明中，蜂巢状结构体优选是交错地密封其两端面成黑白格子状的过滤器结构。
本发明的蜂巢状结构体的制造方法和蜂巢状结构体，在使用在蜂巢状结构体的制造过程中产生的来自蜂巢状结构体的初始原料的回收物制造蜂巢状结构体时，具有与使用原来的初始原料的场合相同程度的低热膨胀性和气孔率，同时可以提高成品率和大幅度降低费用。
本发明的蜂巢状结构体的制造方法，作为初始原料的一部分，使用在蜂巢状结构体的制造过程中产生的来自初始原料的回收物再生的再生原料，再生原料被粉碎至平均粒径为10～2000μm，且平均粒径为2800～100000μm的粒子为0～10重量％。
这是因为，如果将再生原料粉碎到平均粒径小于10μm，不仅粉碎效率差，费用增加，而且粉碎设备的磨耗会增大，并有可能杂质的混入会增多。
另外，在再生原料内，如果平均粒径为2800～100000μm的粒子超过10重量％，在混炼、土炼工序中，再生原料不能充分溶解，成型时堵塞喷嘴，不仅在得到的蜂巢成形体中有可能产生单元缺陷，而且，烧成后得到的蜂巢状结构体(烧成体)的热膨胀率(CTE)变高。
此时，本发明中，更优选再生原料的平均粒径为50～1000μm，粒径0.1～45μm的粒子为1～20重量％，并且粒径1400～100000μm的粒子为0～10重量％。
这是由于，尤其是作为柴油机颗粒过滤器基体的情况，在再生原料内平均粒径为0.1～45μm的粒子超过30重量％时，得到的柴油机颗粒过滤器的平均气孔直径变小。
另外，本发明中，蜂巢状结构体的制造过程中的初始原料中，再生原料的含量优选为1～70重量％。
这是因为，要是再生原料超过70重量％，由于粉碎原料粒子的反应性变得异常，热膨胀率可能会变大。
进一步，本发明中，在蜂巢状结构体的制造过程中产生的来自蜂巢状结构体的初始原料的回收物，优选是未烧成的干燥物。
这是因为，在制造堇青石材质的蜂巢状结构体时，作为再生原料，使用堇青石化原料是必要的、不可缺少的。
另外，制造碳化硅材质的蜂巢状结构体时，再生原料，无论是未烧成的干燥物还是烧成物都没有关系。
进一步，上述回收物是未干燥物时，优选充分干燥后使用。
由上述可知，本发明的蜂巢状结构体的制造方法，在使用在蜂巢状结构体的制造过程中产生的来自蜂巢状结构体的初始原料的回收物制造蜂巢状结构体时，具有与使用原来的初始原料时相同程度的低热膨胀性和气孔率，同时可以提高成品率和大幅度降低费用。
另外，本发明的蜂巢状结构体的制造方法，不仅可以用作载附净化排气中的有害物质的催化剂成分(排气净化用)的催化剂载体，也可以用作是将蜂巢状结构体的两端密封成黑白格子状的过滤器结构的柴油机颗粒过滤器。
本发明的蜂巢状结构体的制造方法，可以良好地适用于为捕集除去柴油机排气那样的含尘流体中所含有的粒子状物质的过滤器(柴油机颗粒过滤器)、或作为载附用于净化排气中的有害物质的催化剂成分(排气净化用)的催化剂载体的制造。
具体实施方式
以下，根据实施例更详细地说明本发明，但本发明不限定于这些实施例。
(实施例1～3、对照例1和对照例2、参考例1)
用锤击式粉碎机，粗粉碎使用了柴油机颗粒过滤器用的堇青石化原料的蜂巢状干燥体，用辊式破碎机粉碎，根据需要进行过筛，分别得到表1中记载的再生原料。接着，相对于70重量％的堇青石化原料，分别准备添加了30重量％再生原料的初始原料，加入粘合剂，用螺旋桨剪切混合器混合3分钟，加入造孔材料，用螺旋桨搅拌混合器混合3分钟，再喷雾添加水，混合3分钟，用∑型捏合机混炼60分钟，得到坯土。用真空土练机将得到的坯土、成形筒状坯土，用活塞式挤出成形机成形为蜂巢形状。微波干燥得到的蜂巢成形体，再热风干燥、得到蜂巢干燥体。将得到的蜂巢干燥体切断为确定的尺寸，交错地密封使堇青石化原料浆料化的密封材料成黑白格子状，在1420℃下烧成6小时，分别得到柴油机颗粒过滤器(单元结构：加强筋0.3mm、单元数：47单元/cm3、尺寸：Φ229mm×L254mm)。
另外，将100％的柴油机颗粒过滤器用的堇青石化原料作为初始原料，用与上述相同的制造方法得到柴油机颗粒过滤器(参考例1)。表1表示得到的柴油机颗粒过滤器的特性。
再者，柴油机颗粒过滤器用的堇青石化原料，使用的是10～30重量％的平均粒径为5～10μm的高岭土、37～41重量％的平均粒径为20～30μm的滑石、10～20重量％的平均粒径为2～5μm的氢氧化铝、10～20重量％的平均粒径4～8μm为的氧化铝、5～20重量％的平均粒径为20～50μm的熔融二氧化硅或石英的组合物。
表1
                再生原料的粒度分布                    蜂巢特性
  平均粒径(μm)   0.1～45μm(重量％)   1400～100000μm(重量％)   2800～100000μm(重量％)   平均气孔率(μm)   气孔率(％)   热膨胀系数(×10-6/℃)   单元缺陷数(个)
实施例1 100 20 0.5 0.0 22 59 0.6 0
实施例2 500 4 1.0 0.0 23 59 0.6 0
实施例3 1000 2 10.0 4.0 24 60 0.6 0
对照例1 7 92 0.0 0.0 14 58 0.8 0
对照例2 3200 1 73.0 57.0 27 65 0.8 6
参考例1 - - - - 23 59 0.6 0
(实施例4～6、对照例3和对照例4、参考例2)
用辊式破碎机，粉碎使用了汽油发动机排气净化用的堇青石化原料的蜂巢干燥体，用破碎机粉碎，根据需要进行过筛，分别得到表2中记载的再生原料。接着，相对于70重量％的堇青石化原料，分别准备添加了30重量％再生原料的初始原料，加入粘合剂、用螺旋桨搅拌混合器混合5分钟，再喷雾添加水，用螺旋桨搅拌混合器混合5分钟，用双轴连续成形机成形为蜂巢形状。微波干燥得到的蜂巢状成形体，再热风干燥、得到蜂巢状干燥体。将得到的蜂巢状干燥体切断为确定的尺寸，在1420℃下烧成4小时，分别得到蜂巢状结构体(单元结构：加强筋0.05mm、单元数：140单元/cm3、尺寸：Φ103mm×L129mm)。
另外，将100％的汽油发动机排气净化用的堇青石化原料作为初始原料，用与上述相同的制造方法，得到蜂巢状结构体(参考例2)。表2表示得到的蜂巢状结构体的特性。
再者，汽油发动机排气净化用的堇青石化原料，使用的是0～40重量％的平均粒径为2～10μm的高岭土、37～41重量％的平均粒径为5～20μm的滑石、0～25重量％的平均粒径为0.5～5μm的氢氧化铝、0～25重量％的平均粒径为2～8μm的氧化铝、0～25重量％的平均粒径为3～20μm的熔融二氧化硅或石英的组合物。
表2
             再生原料的粒度分布                   蜂巢特性
  平均粒径(μm)   0.1～45μm(重量％)  1400～100000μm(重量％)  2800～100000μm(重量％)   平均气孔率(μm)   气孔率(％)   热膨胀系数(×10-6/℃)   单元缺陷数(个)
实施例4 10 90 0.0 0.0 3 34 0.6 0
实施例5 500 5 2.0 0.5 3 34 0.5 0
实施例6 2000 1 17.0 10.0 3 34 0.5 0
对照例3 6 93 0.0 0.0 3 34 0.8 4
对照例4 3300 1 25.0 16.0 12 39 0.8 12
参考例2   -   -  -  -   3   34   0.5   0
再生原料的粒度分布测定，用以下方法进行。
对于大于等于45μm的粒子，根据JIS的标准进行测定。
对于小于等于45μm的粒子，根据用激光反射法的粒度分布测定计(堀場製作所制製：LA-910)测定。
另外，用以下所示的测定方法测定蜂巢特性
(1)平均气孔率
用マィクロメリティックス社制的水银压入式气孔测定计测定细孔分布、平均孔径。
(2)气孔率
将堇青石的真比重定为2.52g/cc，从全部细孔的容积、计算气孔率。
(3)热膨胀系数
将蜂巢状烧成体在流动方向切开，测定40～800℃的热膨胀系数。
(4)单元缺陷数
连续整形50个蜂巢状结构体，数出第51个蜂巢状结构体的每一个的单元缺陷数。
(考察：实施例1～3、对照例1和对照例2、参考例1)
如表1所示，即使和参考例1相比，实施例1～3所得到的蜂巢特性也不逊色，良好。
另一方面，对照例1中，可以认为因为将柴油机颗粒过滤器用原料微粉碎到平均粒径至7μm，所以蜂巢状结构体的平均气孔直径变得小到14μm。另外，其热膨胀系数，变大到0.8×10-6/℃，可以认为，由于微粉碎，原料粒子的反应性变得异常的缘故。
对照例2中，因为再生原料是粗粒，所以在混炼、土炼中，再生原料不能充分溶解，平均气孔直径、气孔率和热膨胀系数变大，发生单元缺陷。
(考察：实施例4～6、对照例3和对照例4、参考例2)
如表2所示，即使和参考例2相比，实施例4～6所得到的蜂巢特性也不逊色，良好。
另一方面，对照例3中，可以认为，由于微粉碎引起设备的磨耗，磨耗粉混入而发生单元缺陷。另外，其热膨胀系数，由于微粉碎，原料粒子的反应性变得异常而增大。
对照例4中，因为与对照例2同样地是再生原料粗粒，所以不能充分溶解，平均气孔直径、气孔率和热膨胀系数变大，发生单元缺陷。

Claims (6)

1.一种蜂巢状结构体的制造方法，所述蜂巢状结构体的制造方法使用在蜂巢状结构体制造过程中产生的来自蜂巢状结构体的初始原料的回收物再生的再生原料作为初始原料的一部分，其特征在于，该再生原料被粉碎至平均粒径为10～2000μm，且平均粒径为2800～100000μm的粒子为0～10重量％。
2.如权利要求1所述的蜂巢状结构体的制造方法，所述再生原料被粉碎至平均粒径为100～1000μm，平均粒径为0.1～45μm的粒子为1～20重量％，并且粒径为1400～100000μm的粒子为0～10重量％。
3.如权利要求1或2所述的蜂巢状结构体的制造方法，所述回收物是未烧成的干燥物。
4.如权利要求1～3任意一项所述的蜂巢状结构体的制造方法，所述蜂巢状结构体是堇青石材质。
5.如权利要求1～4任意一项所述的蜂巢状结构体的制造方法，所述蜂巢状结构体是交错地密封其两端面成黑白格子状的过滤器结构。
6.一种蜂巢状结构体，其特征在于，以权利要求1～5任意一项所述的制造方法制造。
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