CN102123966A - 新型混合含水高岭土产物 - Google Patents

新型混合含水高岭土产物 Download PDF

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CN102123966A
CN102123966A CN2009801320682A CN200980132068A CN102123966A CN 102123966 A CN102123966 A CN 102123966A CN 2009801320682 A CN2009801320682 A CN 2009801320682A CN 200980132068 A CN200980132068 A CN 200980132068A CN 102123966 A CN102123966 A CN 102123966A
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S·马图尔
M·B·西格曼
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Abstract

本发明涉及一种混合含水高岭土产物，其包含片状粗高岭土和含水细高岭土。所述混合高岭土产物适合用作形成堇青石产物的原料组分。

Description

新型混合含水高岭土产物
本申请要求于2008年8月19日提交的美国临时申请序列号61/090024的优先权。
技术领域
本发明涉及一种在特定应用中用作粗制产物的高岭土产物。特别地，本发明涉及一种在堇青石陶瓷蜂窝的形成和烧结中用作原料组分的混合含水高岭土产物。
背景技术
堇青石(Mg2[Al4Si5O18])陶瓷是用于车用催化剂基材、柴油机微粒过滤器应用以及其它高温制品(例如NOx吸附基材、催化剂基材和蜂窝制品)的优选材料，这是由于堇青石陶瓷的低生产成本和例如低热膨胀系数(CTE)和抗热冲击的物理特性的结合。堇青石基材通常是由诸如滑石和高岭土的天然存在的矿物来制备，原因是这些矿物具有低成本和高纯度。堇青石材料通常是通过将原料混合而制成的，这些原料可包括滑石、氧化铝、氢氧化铝、高岭土和二氧化硅。然后可将所述原料与粘结剂(例如甲基纤维素)和润滑剂(例如硬脂酸钠)混合来形成塑性混合物。然后将该塑性混合物成型为生坯并进行烧结。
堇青石晶体结构由四面体的六边形环构成，该四面体通过五个硅原子和一个铝原子在六边形环的每个交点接合。六边形环通过其它的铝四面体和镁八面体连接在一起，从而使得每个单位晶胞有两个沿晶体结构的c轴取向的间隙空位。参见：B.P.Saha，R.Johnson，I.Ganesh，G.V.N.Rao，S.Bhattacharjee，T.R.Mahajan；Materials Chemistry and Physics，67(2001)，140-145。随着温度增加，该间隙空位导致沿着晶体结构的c轴收缩和沿着a轴和b轴膨胀。参见：R.J.Beals，R.L.Cook，J.Am.Ceram.Soc.，35(2)，(1952)，53-57。由堇青石晶体结构引起的各向异性CTE通过将陶瓷内单个晶体的c轴取向为挤出方向而为工程师提供机会，以获得改善的堇青石蜂窝。已经观察到堇青石晶体取向使陶瓷蜂窝的整体CTE显著净减少。参见：I.M.Lachman，R.M.Lewis，1975年5月27日的美国专利No.3,885,977；和R.Johnson，I.Ganesh，B.P.Saha，G.V.Narasimha Rao，Y.R.Mahajan，J.Mater.Sci.，38(2003)，2953-61。
为了使堇青石晶体在陶瓷中定向，可以使用片状原材料。特别地，滑石和高岭土具有片状晶体结构，当在高压下通过挤出模时，片状晶体结构可优先平行于挤出方向地定向。含水高岭土的分层可用来增加粘土的片状性，从而使得在挤出过程中增加了对齐性。然后生坯的烧结使得具有在蜂窝结构内堇青石晶体的优先取向的陶瓷形成，所述蜂窝结构相对于挤出方向沿着c轴取向。参见I.M.Lachman等人，1988年9月20日的美国专利No.4,772,580。虽然滑石和高岭土在烧结的堇青石晶体结构的取向中都发挥作用，但是由于高岭土提供了生坯内有序Al的唯一来源，所以高岭土被认为是最重要的贡献者。由于Si来源于滑石和高岭土原料源，并且Mg(以滑石作为来源)占了最终堇青石晶体的较小的原子和重量百分比，所以预期Al(来自高岭土)对于最终堇青石晶体结构的贡献最大。参见Saha等人。
制备高度有序的堇青石基材的一个缺点是沿蜂窝中的轴向和横向的热膨胀的差异会变得很大，以致于会产生裂缝，从而降低了抗热冲击性能。参见Saha等人。虽然这是涉及催化剂基材的问题，但是对于制备用于柴油微粒过滤器应用的蜂窝来说尤其重要，其中增加的孔隙率降低了所得陶瓷的抗冲击性能。此外，平行于基材轴向的高度取向的原料的挤出降低了生坯的强度，从而使得生坯松垂，特别是在薄壁应用中。为了缓解这些问题，煅烧的粘土往往必须结合分层含水粘土而添加。虽然这种添加使颗粒的对齐性缓和而提供了生坯内的强度，但却以烧结陶瓷内堇青石晶体的对齐性的降低和由此所得的热膨胀系数的减小为代价。特别是与分层含水粘土相比，通过煅烧制备的较粗颗粒的片状性较差。
发明内容
本发明涉及一种混合含水高岭土产物，其包含以直径表示平均粒度小于2μm的片状高岭土和以直径表示平均粒度小于1μm的含水细高岭土，这些可以通过Sedigraph 5100测量。在一个实施方式中，所述片状高岭土是分层高岭土。所述高岭土产物可以在堇青石陶瓷蜂窝的形成和烧结中用作原料组分。
本发明还涉及一种形成混合含水高岭土产物的方法，其包括将作为细组分的从第三纪原沉积物(tertiary crude deposits)开采的粘土和作为粗组分的白垩纪粘土或次生粘土混合。混合的高岭土产物具有总颗粒质量，其中通过Sedigraph 5100测量，总颗粒质量的约75％或更多小于2μm，并且总颗粒质量的超过约55％小于1μm，并且该混合的高岭土产物适于改进的堇青石制造。所述方法包括将粗组分和第三纪细组分混合，其中所述粗组分是颗粒质量的少于85％的粒度小于2μm；在所述第三纪细组分中，样品质量的95％或更多粒度小于1μm，且超过85％的样品的粒度小于0.5μm。
具体实施方式
本发明涉及一种可以在堇青石陶瓷蜂窝的烧结中用作原料组分的混合含水高岭土产物。所述混合产物由片状含水粗高岭土和含水细高岭土构成。这两种原料的组合被认为通过建立机制来控制最终产物中堇青石晶体定向程度而增强堇青石蜂窝的热机械性能。
细粘土与较大的分层粘土结合使用具有若干优点。细粘土可用于在挤出过程中使分层高岭土和滑石的定向缓和，使得定向的堇青石晶体结构保持低的热膨胀系数，并使陶瓷蜂窝在轴向和横向的各向异性热膨胀程度最小化。这会降低通常在正常的催化转化器或过滤操作中所观察到的与温度变化相关的微破裂程度。细粒度粘土还使得颗粒在生坯内的填充得到改善。含水较细粘土会填充在其它煅烧粘土不能填充的较大原料晶体之间的空隙。在生坯内的颗粒填充的改善会在干燥和烧制基材之前增强生坯强度并消除产物变形。
理想的是，堇青石前体在生坯内更均匀地分布，这可能通过添加含水细高岭土组分来实现。提高的均质性会使得前体到堇青石的转化得到改善，并限制了晶体结构内杂质相的形成(这会提高整个陶瓷的热膨胀系数)。与含水较细粘土相关的增大的表面积和降低的结晶度也将具有较低的反应温度，这使得基材的温度降低以及烧制时间减少，同时不会影响到堇青石的整体转换。这样会降低与产物制备相关的能源成本。
本发明的一个实施方式是结合使用片状(但不必是分层的)含水粗高岭土组分和含水细高岭土组分。在该实施方式中，细高岭土会在堇青石成型混合的挤出过程中起到同样的缓和片晶定向的作用，但如果使用非分层的粗组分，则细组分相对于粗组分的比例会降低，以对使用非分层的(较少片状)粗组分加以补偿。
在本发明的另一个实施方式中，混合含水高岭土产物由下述材料的掺混物构成：(1)平均粒径小于2μm的分层含水高岭土(粗高岭土组分)，(2)平均粒径小于1μm的含水细高岭土(细高岭土组分)。粒度已经使用Micrometrics Sedigraph 5100型仪器测得。粗高岭土组分与细高岭土组分的重量比可在约10∶90至约90∶10的范围内，或者在约50∶50至约90∶10的范围内，或者在约70∶30至约90∶10的范围内。粗高岭土组分与细高岭土组分重量比的精确选择将取决于最终产物中所需的组成(即，高岭土掺混物的精确比例将取决于其它原料和精确量，包括制备堇青石中所用批次)，和最终产物所需的特性(例如提高的热膨胀系数、增加的尺寸精度，降低的开裂趋向、整体孔隙率以及孔径)。无需过度试验，本领域的技术人员会知道，所需的粗高岭土组分与细高岭土组分的比例取决于制备堇青石所用的其它原料。粗高岭土组分和细高岭土组分的混合可发生在高岭土开采和加工的任何点。这包括在最初的准备过程中、喷雾干燥之前、喷雾干燥之后或者作为浆液形式的产物将各原料组分混合。只要最终结果是添加两种高岭土组分(这将形成具有本文所述的特性的掺混物)，则粗和细高岭土组分也就能够以单独的组分添加到堇青石原料中。
本发明的另一个实施方式是由第三纪原沉积物开采的粘土作为掺混物的细组分的用途，其与白垩纪粘土或次生粘土结合使用。高岭土原沉积物具有反映其形成时期的物理特性。第三纪原沉积物的尺寸通常较细，具有不同的微量元素状况，例如较高的Fe2O3含量，并且具有比在其它时期沉积的粘土更高的密度。基于第三纪沉积物的粘土由被侵蚀并在37至53百万年前再沉积的白垩纪粘土(最初沉积于65至136百万年前)构成。由分别比75％的粒径为2μm和55％的粒径为1μm(通过Sedigraph 5100测量)更细的粗高岭土和第三纪高岭土构成的掺混物适于改善的堇青石制备。满足这些标准的掺混样品已经通过将分层粗组分与第三纪细组分混合而制备，在所述分层粗组分中，总颗粒质量的低于85％粒度小于2μm；在所述第三纪细组分中，样品质量的95％或更多粒度小于1μm，并且细组分样品的高于85％粒度小于0.5μm。为了制备高性能的堇青石，混合高岭土样品的杂质状况应当满足以下要求：含有少于0.1％的Na2O、少于0.25％的K2O、少于1.75％的TiO2、少于0.6％的Fe2O3、少于0.1％的CaO和少于0.1％的P2O5。
实施例1
实施例1包括若干样品，它们由购自BASF公司的高岭土制备部门的细粒度高岭土和分层粗高岭土流的掺混物制备。分层粗高岭土流源自中佐治亚州地区的两种不同的粗高岭土源。将这些样品标为粗#1和#2。将粗样品#1(～56％的固体)分层，用酸和明矾聚集，过滤并用聚丙烯酸酯分散剂再分散。将粗样品#2(～54％的固体)分层，由于高固体加工，粗样品#2除了添加聚丙烯酸酯之外不需要进行进一步处理。细粘土由开采自中佐治亚州地区的第三纪高岭土(T1)和开采自东佐治亚地区的第三纪高岭土(T2)构成。对两种第三纪高岭土都用酸和明矾进行聚集，过滤，并用聚丙烯酸酯分散剂再分散。各样品通过将分层的和细粒度高岭土流掺混而制备。样品#1包含90重量％的粗#1掺混物和10重量％的T1。样品#2包含90重量％的粗#2和10重量％的T1。样品#3包含90重量％的粗#1和10重量％的T2。样品#4包含90重量％的粗#2和10重量％的T2。表1记载了所制备的四个共混样品的元素分析。表2记载了掺混物以及所用的分层粗高岭土和含水细高岭土组分中的各自的粒度分布。
表1
Figure BDA0000047057590000061
表2
Figure BDA0000047057590000062
实施例2
实施例2涉及本发明的另一个实施方式。掺混物是用含水细高岭土和分层粗高岭土制备的，其中调节掺混物比例以增加细组分。样品是使用在掺混之前被分层的粗高岭土制备的。细高岭土源自从中佐治亚地区开采的第三纪高岭土原沉积物，对该细高岭土用酸和明矾进行聚集，过滤，并用聚丙烯酸酯分散剂再分散。样品#5包含70重量％的分层粗高岭土掺混物和30重量％的中佐治亚地区的第三纪高岭土。表3记载了由该样品获得的元素分析，表4显示了所得的粒度分布。
表3
  样品编号   ％SiO2  ％Al2O3   ％Na2O   ％K2O   ％TiO2  ％Fe2O3   ％CaO   ％MgO   ％P2O5   ％SO3   ％LOI
  样品5   44.8   38.7   0.026   0.08   1.18   0.44   0.04   0.03   0.08   0.05   14.44
表4
Figure BDA0000047057590000071
虽然已经结合优选实施方式详细描述了本发明，但根据前面的描述，对于本领域技术人员来说，多种替代、修改和变型将是显而易见的。因此，应当认为，所附权利要求书将涵盖任何落入本发明真实范围和实质内的这些替代、修改和变型。

Claims (20)

1.一种混合含水高岭土产物，其包含：
a)片状粗高岭土；和
b)含水细高岭土。
2.根据权利要求1所述的高岭土产物，其中所述片状粗高岭土具有以直径表示小于2μm的平均粒度，并且所述含水细高岭土具有以直径表示小于1μm的平均粒度。
3.根据权利要求2所述的高岭土产物，其中所述片状粗高岭土为分层高岭土。
4.根据权利要求2所述的高岭土产物，其中所述粗高岭土组分和细高岭土组分之间的重量比在约10∶90和约90∶10之间。
5.根据权利要求2所述的高岭土产物，其中所述粗高岭土组分和细高岭土组分之间的重量比在约50∶50和约90∶10之间。
6.根据权利要求2所述的高岭土产物，其中所述粗高岭土组分和细高岭土组分之间的重量比在约60∶40和约90∶10之间。
7.根据权利要求1所述的高岭土产物，其中所述粗高岭土组分是白垩纪粘土或次生粘土，并且所述细高岭土组分是从第三纪原沉积物开采的粘土。
8.根据权利要求7所述的高岭土产物，其中所述从第三纪原沉积物开采的粘土具有总颗粒质量，使得通过Sedigraph 5100测量，超过约75％的颗粒小于2μm，并且超过约55％的颗粒小于1μm。
9.根据权利要求7所述的高岭土产物，其中所述混合高岭土产物的杂质状况为：小于0.1重量％的Na2O、小于0.25重量％的K2O、小于1.75重量％的TiO2、小于重量0.6％的Fe2O3、小于0.1重量％的CaO和小于0.1重量％的P2O5。
10.根据权利要求9所述的高岭土产物，其中所述基于第三纪原沉积物的高岭土组分和所述基于白垩纪或次生层的高岭土组分之间的重量比在约90∶10和约10∶90之间。
11.根据权利要求9所述的高岭土产物，其中所述基于第三纪原沉积物的高岭土组分和所述基于白垩纪或次生层的高岭土组分之间的重量比在约50∶50和约10∶90之间。
12.根据权利要求9所述的高岭土产物，其中所述基于第三纪原沉积物的高岭土组分和所述基于白垩纪或次生层的高岭土组分之间的重量比在约40∶60和约10∶90之间。
13.根据权利要求3所述的高岭土产物，其中
a)所述分层粗高岭土包含小于2μm的总颗粒质量的少于约85％；和
b)所述细高岭土包含粒度小于1μm的质量的约95％或更高和粒度小于0.5μm的质量的超过85％。
14.根据权利要求13所述的高岭土产物，其中所述细高岭土是从第三纪原沉积物开采的。
15.根据权利要求14所述的高岭土产物，其中所述第三纪高岭土具有下述总颗粒质量：通过Sedigraph 5100测量，超过约75％小于2μm，超过约55％小于1μm。
16.一种制备堇青石的方法，包括：将包含混合含水高岭土产物的堇青石前体混合、挤出和烧结，所述混合含水高岭土产物包含：
a)片状粗高岭土；和
b)含水细高岭土。
17.根据权利要求16所述的方法，其中
a)所述片状高岭土组分具有以直径表示小于2μm的平均粒度；和
b)所述细高岭土组分具有以直径表示小于1μm的平均粒度。
18.根据权利要求17所述的方法，其中所述片状高岭土为分层高岭土。
19.根据权利要求16所述的方法，其中所述粗高岭土组分和所述细高岭土组分之间的重量比在约50∶50和约90∶10之间。
20.根据权利要求16所述的方法形成的堇青石产物。
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