CN100386150C - 一种陶瓷催化剂载体、微粒捕集器和微粒捕集装置及其制备方法 - Google Patents

一种陶瓷催化剂载体、微粒捕集器和微粒捕集装置及其制备方法 Download PDF

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CN100386150C
CN100386150C CNB2005100109679A CN200510010967A CN100386150C CN 100386150 C CN100386150 C CN 100386150C CN B2005100109679 A CNB2005100109679 A CN B2005100109679A CN 200510010967 A CN200510010967 A CN 200510010967A CN 100386150 C CN100386150 C CN 100386150C
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clay
carborundum
carrier
ceramic catalyst
catalyst carrier
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CN1915520A (zh
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陈庆华
李电益
李�一
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Yunnan Filter Environmental Technology Co., Ltd.
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YUNNAN FILTER ENVIRONMENTAL TECHNOLOGY Co Ltd
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Priority to CNB2005100109679A priority Critical patent/CN100386150C/zh
Priority to EP06775410.1A priority patent/EP1925353B1/en
Priority to US12/063,813 priority patent/US8114184B2/en
Priority to JP2008526359A priority patent/JP2009504389A/ja
Priority to PCT/CN2006/002092 priority patent/WO2007019801A1/zh
Priority to KR1020087005712A priority patent/KR101310787B1/ko
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Abstract

一种陶瓷催化剂载体和该载体构成的微粒捕集装置及其它们的制备方法。本发明提供了一种以碳化硅为基体的蜂窝陶瓷催化载体和壁流式过滤装置，其以碳化硅、粘土、粘接剂、润滑剂、水为主要原料，粘接剂为面粉加水制作的糊精，润滑剂为机油、将原料粉末、粘接剂和润滑剂混合制成泥团；经挤压形成蜂窝型陶坯，交叉封孔形成壁流式结构的过滤单元，经高温烧结热处理得到的成品；壁流式过滤单元可以按设计生产成不同多面体或曲边多面柱体，组合、粘接后形成车用过滤装置。本发明解决了柴油车和其余机动车的颗粒污染问题，有效减少汽车特别是柴油车尾气对环境的污染。

Description

一种陶瓷催化剂载体、微粒捕集器和微粒捕集装置及其制备方法
技术领域
本发明涉及一种陶瓷催化剂载体、微粒捕集器和微粒捕集装置。更具体地说，本发明涉及一种汽车或工业废气催化-净化装置采用的SiC基陶瓷催化剂载体及壁流式微粒捕集装置。同时，本发明还涉及所述的载体和捕集装置的制备方法。
背景技术
现代社会的发展使汽车保有量出现了大幅度增长，而尾气排放所产生的污染也大量增加。汽车集中的发达地区，特别是大城市，尾气排放产生的污染已占这些地区大气污染的50％～60％。随着人们对生存环境的重视，降低汽车尾气排放，治理尾气污染已成为国内外关注的话题。从技术上而言，降低汽车尾气排放的措施有机前措施、机内措施和机后措施等三种方法，目前国内外主要是采用上述三种措施结合的方法治理尾气，随着尾气排放标准逐渐提高，机外措施就显得更加重要，即用催化净化的方法来降低尾气污染物的排放。汽车尾气催化净化器主要由外壳、载体和催化剂三部分组成。催化剂载体及微粒捕集装置的性能直接影响着催化剂的活性，影响净化效果。
现有技术中，日本NGK公司和法国IBIDEN公司提出用纯的碳化硅作为催化剂载体(见欧洲专利EP1142619A1)，其制备方法采用挤压方式生产，由于纯碳化硅载体生产的特殊性，采用分体组合的方式构成整体，并且采用世界通用的交叉封孔的方法形成壁流式设计构成，该载体也在柴油车微粒捕集再生中得到了应用。纯碳化硅载体在高温下耐火性能突出，可以达到2200℃，在柴油车碳烟捕集和再生过程中有明显的高温优势。但是，该载体由于烧结温度高，生产工艺控制复杂，能耗太高，因此，价格居高不下，对该载体的广泛应用形成了极大的阻力，特别是在发展中国家，推广使用该技术非常困难，因此，产品性价比的提高是本技术领域一个急待解决的技术难题。
发明内容
本发明的目的在于针对现有技术的不足，提供一种以碳化硅为基础原料，普通粘土为粘结料的陶瓷催化剂载体、一种由该载体构成的壁流式微粒捕集器和微粒捕集装置。同时，本发明还提供所述载体、捕集器和微粒捕集装置的制备方法。
本发明的目的通过下述技术方案予以实现。
本发明提供了一种陶瓷催化剂载体，该载体是由下述重量份数的原料制成的：碳化硅1，粘土0.05～0.5，面粉0.1～0.35，机油0.025～0.05，水0.2～0.35；载体为4孔～62孔/平方厘米的蜂窝型，蜂窝体壁厚为0.2～1.2mm，其微孔孔隙率为40％～70％，通孔率＞30％，微孔孔隙平均半径为1～50μm。
其中，所述的粘土为工业粘土或颜料级粘土；所述的机油是重质馏份润滑油和合成润滑油中的一种；或者是它们的混合物。
本发明提供了所述陶瓷催化剂载体的制备方法，该方法采用以下步骤：
(1)按配比称量各组份：碳化硅1，粘土0.05～0.5，面粉0.1～0.35，机油0.025～0.05，水0.2～0.35；
(2)将碳化硅用震动筛筛分，采用两种以上颗粒度不同的碳化硅搭配，两种颗粒的颗粒度搭配以相差200目为好，例如：采用200目和400目碳化硅进行搭配，200目粉与400目粉的混合重量比为1∶3；加入粘土，并充分混合均匀；然后加入机油，在搅拌机内充分搅拌，待用；
(3)将面粉和水在常温下混合成浆，在65℃～100℃下熟化成糊精；
(4)将糊精和步骤(2)的所得物在搅拌机内混合，搅拌1～3小时；
(5)对泥料进行混炼和筛制，使泥料充分均匀；
(6)用模具挤压成型，形成4孔～62孔/平方厘米的蜂窝型陶瓷素坯；经室温干燥，叉孔封堵；
(7)以＜5℃/mi n的速度加温到600℃～900℃保温6～12小时；然后将温度升到1250℃～1400℃保温4～12小时，随炉冷却到室温出窑，制得所需的陶瓷催化剂载体。
本发明深入***的试验结果表明：
(1)烧成后的产品的微孔孔隙率在40％～70％，其中开孔率＞30％，微孔孔隙平均半径在1～50μm。如果微孔孔隙平均半径高于50μm，那么，微粒就会泄漏，达不到捕集效果；微孔孔隙半径小于1～10μm，那么背压会成倍增加，对发动机的功率影响极大；最佳的平均孔隙半径约为10～30μm；
(2)烧成后的壁流式蜂窝陶瓷催化剂载体壁厚约为0.2～1.2mm，壁厚＞1.2mm则气孔通孔率较小，背压会成倍增加，对发动机的功率影响较大；壁厚＜0.2mm则壁面机械强度会相应降低，因此也会影响使用；最佳壁厚在0.2～0.6mm之间；
(3)碳化硅级配对孔隙率的形成有重要影响，一般应该采用两种以上颗粒度不同的碳化硅，颗粒度搭配应该两两相差200目为好，如采用200目与400目碳化硅进行适当搭配会取得恰当的效果，以上的叙述仅仅是一个范例，搭配方法不仅此一种；碳化硅的量应该占总有效成分的50％～95％；
(4)粘土应该选用工业粘土或颜料级粘土作为对象，应该选择＞200目的粘土作为高温粘结相，粘土的使用量应该根据碳化硅的级配选择，应该用模拟的方法选择稍高于渗流径形成的量为好，一般应在5％-50％之间；
本发明还提供了一种微粒捕集器，该微粒捕集器由多个所述的陶瓷催化剂载体采用粘结剂相互粘结而成，所述的粘结剂的重量份组成为：碳化硅1，粘土0.2～1，水玻璃0.06～0.35。
所述的微粒捕集器是方形柱体、跑道形柱体、圆形柱体或者由多面柱体及弧形柱体相互拼装成的光滑形体。
所述的微粒捕集器外部包裹隔热衬垫，并封装于不锈钢外壳内形成尾气微粒捕集装置，应用于柴油汽车发动机尾气微粒捕集和后处理。
该微粒捕集器的应用体积应该和汽车的排量匹配，本发明的试验研究表明最佳的匹配方式为：微粒捕集器的体积是柴油车排量的1～2.5倍。
催化剂载体的再生问题可以采用化学物理方法，如催化连续再生CRT、喷油燃烧、电加热等，这些装置的应用最好和将要采用的汽车、柴油车车载在线检测***(OBD***)联合使用。
本发明提供了一种微粒捕集装置的制备方法，该方法采用以下步骤：
(1)以所述的陶瓷催化剂载体作为组合件，采用几何拼图的方法，将粘结剂均匀涂抹于需要粘结的陶瓷载体组件的表面，粘结成方形柱体、跑道形柱体、圆形柱体或者由多面柱体及弧形柱体相互拼装成的光滑形体；粘结剂的重量份组成为：碳化硅1，粘土0.2～1，水玻璃0.06～0.35；涂层厚度为1～3mm；
(2)所述形体用不锈钢形成外壳模，填入粘料，制成外壳；
(3)将粘结柱体连同不锈钢模送入烘烤炉，从室温加热到120℃烘烤8小时；
(4)脱模并形成初坯，用粘接浆料刷涂表面，干燥成型后制得微粒捕集器；
(5)将催化载体和微粒捕集器用蛭石隔热衬垫包裹；一前一后焊接封装于不锈钢外壳中，并焊接进气管和出气管，形成尾气催化转化、颗粒捕集分解装置。
本发明的基本原理：采用了物理化学研究中的愈渗(渗流)原理，使一个基体为SiC的耐火材料，可以在保持一定的耐火度的前提下，在较低的温度下得以烧成；在降低一定耐火度、同时满足催化或过滤材料的基本要求的前提下，达到节约能源、降低成本、扩大生产、扩充使用范围的目的。基本要求是，作为粘结相使用的粘土的体积或重量比应该接近或适当超过渗流极限，在通常三维材料中该比值应该为5％～50％，该百分比不仅取决于材料种类，还取决于材料的微观结构，对于具体的材料有具体的下限值。应用先进的挤压成型技术形成多孔的蜂窝陶瓷坯体。采用传统的烧结技术，通过调节配方，达到具有适当的耐火、导热、热膨胀、孔隙率和力学机械性能等特殊要求。
与现有技术相比本发明具有以下有益效果：
(1)产品具有以下几个突出的性能特点：①由于采用先进的挤压成型工艺，蜂窝陶瓷载体单位表面积的直孔数众多，可在4～62孔/平方厘米，有利于催化剂和尾气的充分接触。②载体由于用级配和渗流原理，孔壁上形成及其丰富的微细孔(孔的大小和分布可以用粉末级配、粘接剂或造孔剂加以调节)，有利于催化剂的负载，同时也有利于柴油机烟尘的捕集。③用于柴油机烟尘的捕集，还可以定期用化学方法或喷油或电加热的方法除去捕集的烟尘，保证柴油机烟尘捕集器的畅通和有效工作。
(2)使用工业碳化硅和粘土为主要原料，材料来源广泛、价格低廉、成型容易，烧结可使用传统粘土耐火材料烧结设备，大大简化了生产加工过程，得到的陶瓷体不仅多孔，而且导热、孔隙度和机械强度足以用于汽车、化工等行业的催化捕集载体。
(3)产品的耐火度适中、性价比优良。同时，采用世界通用的交叉封孔的方法，形成壁流式微粒捕集器。其制备方法原料丰富，成本低廉，成型容易，烧结工艺合理。
(4)具有十分广泛的应用范围，例如：冶金行业的熔渣过滤、热交换；环境处理问题中的污水过滤及净化等；化工行业中的催化剂载体；航空、航天材料的制备等。本发明提供的以SiC为基本原料的陶瓷催化剂载体首先可用于汽车尾气的处理，并可推广应用于柴油机车的尾气净化问题，用于捕集、分解烟尘及有害气体。本发明有效地减少柴油车以及其它机动车辆尾气对环境的污染。
附图说明
图1是本发明的陶瓷催化剂载体的产品照片；
图2是所述的方形柱体的微粒捕集器的示意图；
图3是所述的圆形柱体的微粒捕集器的示意图；
图4是所述的跑道形柱体的微粒捕集器的示意图；
图5是本发明应用于柴油汽车发动机尾气微粒捕集和后处理时，其尾气催化转化装置的示意图。
在图5中，隔热衬垫1，催化单元2，捕集单元3，不锈钢外壳4，尾气进口5，尾气出口6。
具体实施方式
通过下面给出的具体实施例可以进一步清楚地了解本发明。但它们不是对本发明的限定。
实施例1
以碳化硅、精选粘土、面粉、机油、水为原料，原料的重量份组成为碳化硅1，粘土0.5，面粉0.35，机油0.05，水0.35；碳化硅粉采用200目粉和400目粉以1∶3的比例混合；粘土的颗粒度为1200目。将面粉和水混合成浆，在65℃～100℃下糊化，备用；将碳化硅、粘土和机油在搅拌机内混合1小时，然后加入面粉糊，充分搅拌1小时，形成均匀泥团备用。将泥团用100目筛过筛，然后用壁厚为1.2mm、25孔/平方英寸(25CPS I)的模具挤压，形成57×57×254mm3的样品备用。经过室温干燥，在＜1350℃的隧道窑中烧结，形成成品。产品性能见表1。
表1.样品尺寸：57×57×254mm3，载体型号：MJK-1
  产品化学组成   (α-SiC+粘土)烧结体
  材料密度(g/cm<sup>3</sup>)   3.60
  壁面材料比重(g/cm<sup>3</sup>)   1.40
  载体视在比重(g/cm<sup>3</sup>)   0.70
  单位英寸孔数/壁厚(CPSI/Mi l)   25/47
  背压(mb)   ＜70-200
  微孔分布范围μm   1-50
  开孔率   ＞30％
  耐火度(℃)   1500
  正常使用温度(℃)   -20-1400
实施例2
重复实施例1，有以下不同：原料的重量份组成为碳化硅1，粘土0.15，面粉0.35，机油0.05，水0.35；碳化硅粉采用300目粉和500目粉以1∶3的比例混合；粘土的颗粒度为1000目。
实施例3
重复实施例1，有以下不同：原料的重量份组成为碳化硅1，粘土0.3，面粉0.18，机油0.03，水0.25；碳化硅粉采用400目粉和600目粉以1∶3的比例混合；粘土的颗粒度为200目。
实施例4
重复实施例1，有以下不同：原料的重量份组成为碳化硅1，粘土0.4，面粉0.3，机油0.04，水0.30；碳化硅粉采用250目粉和450目粉以1∶3的比例混合；粘土的颗粒度为800目。
实施例5
以碳化硅、精选粘土、面粉、机油、水为原料，原料的重量份组成为碳化硅1，粘土0.2，面粉0.35，机油0.05，水0.35；碳化硅粉采用200目粉和400目粉以1∶3的比例混合；粘土的颗粒度为1200目。将面粉和水混合成浆，在65℃～100℃糊化后备用；将其余原料在搅拌机内混合2小时，然后加入面粉糊，充分搅拌2小时，形成均匀泥团备用。
将泥团用120目筛过筛，然后用壁厚为1.0mm，25孔/平方英寸(25CPSI)的模具挤压，形成36×36×254mm3的样品备用。
经过室温干燥，交叉堵孔后，在＜1350℃的隧道窑中烧结，形成成品，性能如表2所示。
表2.样品尺寸：36×36×254mm3，载体型号：MJK-2
  产品化学组成   (α-SiC+粘土)烧结体
  材料密度(g/cm<sup>3</sup>)   3.62
  壁面材料比重(g/cm<sup>3</sup>)   1.41
  载体视在比重(g/cm<sup>3</sup>)   0.74
  单位英寸孔数/壁厚(CPSI/Mil)   25/47
  背压(mb)   ＜70-200
  微孔分布范围μm   1-50
  开孔率   ＞30％
  耐火度(℃)   1500
  正常使用温度(℃)   -20-1400
实施例6
以碳化硅、精选粘土、面粉、机油、水为原料，原料的重量份组成为碳化硅1，粘土0.1，面粉0.35，机油0.05，水0.35；碳化硅粉采用220目粉和W28粉以1∶3的比例混合；粘土的颗粒度为1200目。将面粉和水混合成浆，在65-100℃糊化后备用；将其余原料在搅拌机内混合一小时，然后加入面粉糊，充分搅拌1-3小时，形成均匀泥团备用。
将泥团用150目筛过筛，然后用壁厚为0.6mm，120孔/平方英寸(120CPSI)的模具挤压，形成36×36×254mm3的样品备用。
经过室温干燥并交叉封孔后，在＜1350℃的隧道窑中烧结，形成成品，产品性能如表3。
表3.(样品尺寸：36×36×254mm3，载体型号：MJK-3)
  产品化学组成   (α-SiC+粘土)烧结体
  材料密度(g/cm<sup>3</sup>)   3.65
  壁面材料比重(g/cm<sup>3</sup>)   1.48
  载体视在比重(g/cm<sup>3</sup>)   0.78
  单位英寸孔数/壁厚(CPSI/Mil)   120/24
  背压(mb)   ＜70-200
  微孔分布范围μm   1-50
  开孔率   ＞30％
  耐火度(℃)   1500
  正常使用温度(℃)   -20-1400

Claims (8)

1.一种陶瓷催化剂载体，该载体是由下述重量份数的原料制成的：碳化硅1，粘土0.05～0.5，面粉0.1～0.35，机油0.025～0.05，水0.2～0.35；该载体为4孔～62孔/平方厘米的蜂窝型，蜂窝体壁厚0.2～1.2mm，其微孔孔隙率为40％～70％，通孔率＞30％，微孔孔隙平均半径为1～50μm。
2.根据权利要求1所述的陶瓷催化剂载体，其中所述的粘土为工业级粘土或颜料级粘土。
3.根据权利要求1所述的陶瓷催化剂载体，其中所述的机油是重质馏份润滑油和合成润滑油中的一种或者是它们的混合物。
4.一种陶瓷催化剂载体的制备方法，该方法采用以下步骤：
(1)按重量份数配比称量各组份：碳化硅1，粘土0.05～0.5，面粉0.1～0.35，机油0.025～0.05，水0.2～0.35；
(2)将碳化硅用震动筛筛分，采用两种颗粒度相差200目的碳化硅搭配，大颗粒度的碳化硅与小颗粒度的碳化硅的混合重量比为1∶3；加入粘土，并充分混合均匀；然后加入机油，在搅拌机内充分搅拌，待用；
(3)将面粉和水在常温下混合成浆，在65℃～100℃下熟化成糊精；
(4)将糊精和步骤(2)的所得物在搅拌机内混合，搅拌1～3小时；
(5)对泥料进行混炼和筛制，使泥料充分均匀；
(6)用模具挤压成型，形成4孔～62孔/平方厘米的蜂窝型陶瓷素坯；经室温干燥，叉孔封堵；
(7)以＜5℃/分钟的速度加温到600℃～900℃保温6～12小时；然后将温度升到1250℃～1400℃保温4～12小时，随炉冷却到室温出窑，制得所需的陶瓷催化剂载体。
5.一种微粒捕集器，该微粒捕集器由多个陶瓷催化剂载体采用粘结剂相互粘结而成；所述的陶瓷催化剂载体是由下述重量份数的原料制成的：碳化硅1，粘土0.05～0.5，面粉0.1～0.35，机油0.025～0.05，水0.2～0.35；该载体为4孔～62孔/平方厘米的蜂窝型，蜂窝体壁厚0.2～1.2mm，其微孔孔隙率为40％～70％，通孔率＞30％，微孔孔隙平均半径为1～50μm；所述的粘结剂的重量份组成为：碳化硅1，粘土0.2～1，水玻璃0.06～0.35。
6.根据权利要求5所述的微粒捕集器，其特征在于：其形状是方形柱体、圆形柱体或由多面柱体及弧形柱体相互拼装成的光滑形体。
7.一种微粒捕集装置，该装置由权利要求5所述的微粒捕集器外部包裹隔热衬垫，并封装于不锈钢外壳内形成。
8.一种微粒捕集装置的制备方法，该方法采用以下步骤：
(1)采用权利要求1所述的陶瓷催化剂载体作为组合件，采用粘结的方法，将粘结剂均匀涂抹于需要粘结的陶瓷催化剂载体组件的表面，粘结成方形柱体、圆形柱体或由多面柱体及弧形柱体相互拼装成的光滑形体；粘结剂的重量份组成为：碳化硅1，粘土0.2～1，水玻璃0.06～0.35；涂层厚度为1～3mm；
(2)将步骤(1)得到的粘结体用不锈钢形成外壳模，填入粘料，制成外壳；
(3)将粘结体连同不锈钢模送入烘烤炉，从室温加热到120℃烘烤8小时；
(4)脱模并形成初坯，用粘接浆料刷涂表面，干燥成型后制得微粒捕集器；
(5)将催化载体和微粒捕集器用蛭石隔热衬垫包裹；一前一后焊接封装于不锈钢外壳中，并焊接进气管和出气管，形成尾气催化转化、颗粒捕集分解装置。
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