CN111393155A - 一种薄壁大孔径的堇青石蜂窝陶瓷载体及其制备方法 - Google Patents
一种薄壁大孔径的堇青石蜂窝陶瓷载体及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- 229910052878 cordierite Inorganic materials 0.000 title claims abstract description 45
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 title claims abstract description 45
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- 239000000047 product Substances 0.000 claims description 45
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 44
- 239000000377 silicon dioxide Substances 0.000 claims description 43
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 27
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- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
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- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 3
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开一种薄壁大孔径的堇青石蜂窝陶瓷载体,堇青石蜂窝陶瓷载体中堇青石晶相含量>90%,堇青石蜂窝陶瓷载体的中值孔径≥4.3μm,孔隙率≥32.7%,热膨胀系数≤0.35×10‑6/℃,A轴抗压≥5.5MPa。本发明还公开了陶瓷载体的制备方法,包括如下步骤:(1)将无机物料与有机粘结剂干混均匀,得干混物料;(2)在干混物料中加入表面活性剂、润滑剂以及分散剂,湿混,得具有塑性的颗粒;(3)将塑性的颗粒除去杂质后,在抽真空状态下连续挤出;(4)将挤出成型后的半成品采用微波处理,同时进行吸风干燥,切割,烧结后,得蜂窝陶瓷载体。
Description
技术领域
本发明涉及一种车用堇青石蜂窝陶瓷体及其制备方法,具体地,涉及到一种薄壁,大孔径,低膨胀,高强度,且烧成合格率高,利于催化剂涂覆的车用堇青石制品及其制备方法。
背景技术
近年来汽车行业的排放法规不断升级,对污染物排放限制越来越严格,要求后处理***必须对气态污染物氮氧化物(NOx)、碳氢化合物(HC)和一氧化碳(CO) 具有更高的低温转化效率。为获得良好的低温转化能力,需要使用壁厚4mil、 3mil、2mil比热容更低的薄壁蜂窝陶瓷载体。
生产薄壁蜂窝陶瓷载体产品需要降低原材料粒度,但粒度的降低,特别是滑石粒度的降低,会增加产品的热膨胀系数(CTE)(专利CN 108178652A),为此,在原材料中引入勃姆石,但由于勃姆石是亚微米甚至是纳米级的材料,会导致产品的收缩增加,孔径降低到1.5μm左右,如日本特表2001-524452公开的技术,这不利于催化剂的涂覆(通常,孔径≥3μm有利于催化剂涂覆)。因此为增加产品的孔径,专利CN100410206C中采用使用部分粗氧化铝代替勃姆石,同时提高高岭土的粒径的方法提高产品的孔径,产品孔径最大在4.3μm。专利CN 102292309B中引入5-20%左右的造孔剂(玉米淀粉)继续增加产品的孔径,将中值孔径提高到更高的值,为2-10μm。但是通过引入造孔剂不仅会增加产品生产的成本,还会降低产品烧成的合格率,大尺寸的产品如直径≥10.5英寸,高度≥6英寸,甚至无法烧结。
另外严苛的法规除了需要蜂窝陶瓷载体有优良的涂覆性能,还需要蜂窝陶瓷载体具备较低的膨胀系数以应对极冷极热的环境,本公司在之前申请的专利CN 108178652A中披露了一种特殊制法氢氧化铝(水解铝法),粒径D50在0.2μ m-4.0μm,利用该氢氧化铝可以起到降低产品的CTE,同时降低产品的微裂纹数量,制备出低CTE且强度较高,且成本低廉的堇青石蜂窝陶瓷制品的方法。但是该产品的孔径较小约2.5-3.0微米。
发明内容
本专利的目的是披露一种超薄壁、大孔径、低膨胀、高强度、高烧成合格率,且利于催化剂涂覆的车用堇青石蜂窝陶瓷的制备配方与制备工艺。该方法能在较低的生产成本下获得超薄壁(2-4mil),大孔径(4-11μm),低膨胀(≤0.35× 10-6/℃),高强度(A轴抗压≥5.5MPa),且烧成合格率高(≥98.7%)的堇青石蜂窝陶瓷制品。
本发明是通过以下技术方案实现的:
一种薄壁大孔径的堇青石蜂窝陶瓷载体,所述堇青石蜂窝陶瓷载体中堇青石晶相含量>90%,按质量分数计,其化学成分组成为48.0-52.0%的SiO2, 33.8-37.4%的Al2O3,13.0-15.5%的MgO,
所述堇青石蜂窝陶瓷载体的中值孔径≥4.3μm,孔隙率≥32.7%,热膨胀系数≤0.35×10-6/℃,A轴抗压≥5.5MPa。
进一步地,所述堇青石蜂窝陶瓷载体中堇青石晶相含量≥95%,按质量分数计,其化学成分组成为48.0-52.0%的SiO2,33.8-37.4%的Al2O3,13.0-15.5%的MgO,
所述堇青石蜂窝陶瓷载体的中值孔径≥5.4μm,孔隙率至≥34.1%,热膨胀系数≤0.28×10-6/℃,A轴抗压≥8.1MPa。
本发明还公开一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,包括以下操作步骤:
(1)将无机物料与有机粘结剂干混均匀,得干混物料;无机物料按质量分数计包括41.0-43%滑石、3.0-21.9%中空二氧化硅、13.7-27.8%氧化铝、 5.0-19.62%片状氢氧化铝、0-28.3%无机物煅烧高岭土、生高岭土0-14.0%;
(2)在干混物料中加入表面活性剂、润滑剂以及分散剂,湿混,得具有塑性的颗粒;
(3)将塑性的颗粒除去杂质后,在抽真空状态下连续挤出;
(4)将挤出成型后的半成品采用微波处理,同时进行吸风干燥,切割,烧结后,得蜂窝陶瓷载体。
该制备方法中的过筛采用的是湿法过筛,与传统的干法过筛相比,湿法过筛具有粉尘少,环保,低耗能,且效率高等优点;且该生产工艺中采用的是吸风干燥,吸风干燥避免了低沸点有机物大量挥发造成的环境污染,过程充分利用微波排气余热,降低了热能浪费,无微波到烘干干燥的工艺转接,有效控制了蜂窝陶瓷坯体降温到升温过程的能量消耗,工艺过程缩短,有利与生产效率的提高。
进一步地,所述滑石中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述中空二氧化硅的加入量,按质量分数计,优选为3.0-18.0%,中位粒径 D50为≥16μm,最大粒径D100为≤60μm,堆积密度为≤0.6g/cm3,抗压强度为≥20MPa,所述中空二氧化硅模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土的加入量,按质量分数计,优选为5.9-22.7%,煅烧高岭土中位粒径D50为≥6μm,最大粒径D100为≤35μm;
所述生高岭土的加入量,按质量分数计,优选为0-8.0%,中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述氧化铝的加入量,按质量分数计,优选为16.2-23.9%,中位粒径D50 为≥4μm,最大粒径D100为≤25μm;
所述片状氢氧化铝的加入量,按质量分数计,优选为5.0-10.0%,D50为 0.2-4.0μm,所述片状氢氧化铝采用水解铝法制得,具体操作为:采用液氮急速冷却的方法,在106-107K/S的极冷过程中,金属铝表面会产生大量的空位,错位及层错的缺陷,增加金属铝的活性,与水反应后,产生片状,高活性,高纯度,高表面积氢氧化铝,成品中钾、钠元素的总质量含量低于0.1%。
进一步地,所述滑石中位粒径D50优选为≥16μm,最大粒径D100优选为≤ 50μm;
所述中空二氧化硅的加入量,按质量分数计,更优选为6-15%,中位粒径D50 优选为≥18μm,最大粒径D100优选为≤50μm,堆积密度优选为≤0.5g/cm3,抗压强度优选为≥30MPa,所述中空二氧化硅模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土中位粒径D50优选为≥8μm,最大粒径D100优选为≤30μm;
所述生高岭土的加入量,按质量分数计,优选为0-8%,中位粒径D50为≥ 16μm,最大粒径D100为≤50μm;
所述氧化铝中位粒径D50优选为≥6μm,最大粒径D100优选为≤20μm;
所述片状氢氧化铝的D50优选为1.0-3.0μm。
进一步地,所述有机粘结剂为甲基纤维素,羟丙基纤维素以及甲基纤维素衍生物中的任意一种或其组合;加入量为干混物料质量的1-10%,优选的加入量为干混物料质量的4-7%。
进一步地,所述表面活性剂为硬脂酸、硬脂酸镁、硬脂酸铝、月桂酸及油酸中的任意一种,加入量为干混物料质量的0.5-6%,优选为干混物料质量的1-3%。
进一步地,所述润滑剂为植物油或矿物油中的任意一种,其加入量为干混物料质量的0.5-3%,优选加入量为干混物料质量的1-3%。
进一步地,所述分散剂为水或有机分散剂中的任意一种,所述有机分散剂为乙醇,丙酮中的任意一种,其加入量为干混物料质量的20-35%,优选加入量为 22-28%。
由以上的技术方案可知,本发明的有益效果是:
本发明的优点在于优化原材料的粒度级配,选用中位粒径较大,同时控制最大粒径的原材料,如选用中位粒径较大的煅烧高岭土、生高岭土和氧化铝,同时控制原材料的最大粒径不能超过模具的槽宽;同时引入一种球形,中空的二氧化硅,该球形中空二氧化硅中位粒径较大,且最大粒径不超过模具的槽宽,其堆积密度小于实心的二氧化硅,且抗压强度能够耐受过筛以及连续挤出的压力,生产过程中不发生形变、破碎,通过优化选用中位粒径较大的原材料,可以增加堇青石前驱体坯料中的堆积孔隙和孔径,同时烧结过程中可以减少制品的收缩,提高制品的孔径,通过控制原料的最大粒径,如≤50μm,可以减少产品成型过程中的断筋等缺陷;通过引入球形,中空二氧化硅,可以降低堇青石前体坯料的堆积密度,增加堆积的孔隙,在形成堇青石过程中,中空球反应后在熟坯中留下的孔径更大,增大产品的孔径;现有专利使用造孔剂如豌豆淀粉增加产品的孔隙率和孔径,但是有机造孔剂低温快速氧化会引起坯体内外的温度差异,且有机造孔剂的氧化温度往往与前驱体坯料中的粘结剂,表面活性剂等有机物部分重合,加大温度差异,大的温度差异形成的热应力会导致产品在低温阶段开裂,降低烧成的合格率,一般为烧出合格的产品会降低制品低温阶段的升温速率,从而增加制品的生产周期,降低生产效率,本发明中用无机的二氧化硅中空球代替有机造孔剂,其不会在低温阶段氧化放热其反应温度高于前驱体坯料中粘结剂、润滑剂等的氧化温度,降低坯体低温阶段的热应力,提高产品的合格率;关于中空微球可以考虑有机聚合物中空微球和无机中空二氧化硅微球,但是与有机中空微球相比,无机的二氧化硅微球的强度一般较高,在抽真空挤出等加工过程中耐受更大的压力,不会变形、破碎,使得制品的孔径以及孔隙率等参数更为稳定,且提高烧成合格率,另外中空二氧化硅可以作为堇青石形成的原料,是前驱体坯料的骨架,相较于有机中空微球更节约成本。
附图说明
图1为薄壁大孔径的堇青石蜂窝陶瓷载体制备流程图;
图2为陶瓷载体孔径、孔隙率和抗压强度随中空二氧化硅加入量变化;
图3为堇青石蜂窝制品孔分布图片;
图4为堇青石蜂窝制品表面扫描图片。
具体实施方式
下面将结合实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限制本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
本发明孔径和孔隙率都是通过压汞法测定,仪器是麦克默瑞提克(上海)仪器有限公司,生产的AUTOPORE 9500。产品的中值孔径D50是指压入的汞体积占材料孔总体积50%时对应的孔径。
所用原材料的粒径指的是原材料的累积分布的中位粒径,采用激光衍射原理测定,使用的是欧美克的LS-609仪器。
本发明开一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,包括以下操作步骤:
(1)将无机物料与有机粘结剂干混均匀,得干混物料;无机物料按质量分数计包括41.0-43%滑石、3.0-21.9%中空二氧化硅、13.7-27.8%氧化铝、 5.0-19.62%片状氢氧化铝、0-28.3%无机物煅烧高岭土、生高岭土0-14.0%;
(2)在干混物料中加入表面活性剂、润滑剂以及分散剂,湿混,得具有塑性的颗粒;
(3)将塑性的颗粒除去杂质后,在抽真空状态下连续挤出,挤出的蜂窝陶瓷直径≤330.2mm,高度≤254mm,产品的目数在300-900目,壁厚在2-4mil;
(4)将挤出成型后的半成品采用微波处理,同时进行吸风干燥,切割,烧结后,得蜂窝陶瓷载体,其中烧结的升温制度,见表1。
表1蜂窝陶瓷载体烧成升温制度
温度段,℃ | 每段时间(h) | 速率(℃/h) |
室温-500 | 60.0 | 7.5 |
500-550 | 2.0 | 25.0 |
550-600 | 1.8 | 28.0 |
600-1050 | 11.3 | 40.0 |
1050-1150 | 2.0 | 50.0 |
1150-1270 | 1.5 | 80.0 |
1270-1370 | 1.3 | 76.9 |
1370-1430 | 2.0 | 30.0 |
1430-1430 | 8.0 | 0.0 |
进一步地,所述滑石中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述中空二氧化硅的加入量,按质量分数计,优选为3.0-18.0%,中位粒径 D50为≥16μm,最大粒径D100为≤60μm,堆积密度为≤0.6g/cm3,抗压强度为≥20MPa,所述中空二氧化硅模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土的加入量,按质量分数计,优选为5.9-22.7%,煅烧高岭土中位粒径D50为≥6μm,最大粒径D100为≤35μm;
所述生高岭土的加入量,按质量分数计,优选为0-8.0%,中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述氧化铝的加入量,按质量分数计,优选为16.2-23.9%,中位粒径D50 为≥4μm,最大粒径D100为≤25μm;
所述片状氢氧化铝的加入量,按质量分数计,优选为5.0-10.0%,D50为 0.2-4.0μm,所述片状氢氧化铝采用水解铝法制得,具体操作为:采用液氮急速冷却的方法,在106-107K/S的极冷过程中,金属铝表面会产生大量的空位,错位及层错的缺陷,增加金属铝的活性,与水反应后,产生片状,高活性,高纯度,高表面积氢氧化铝,成品中钾、钠元素的总质量含量低于0.1%。
进一步地,所述滑石中位粒径D50优选为≥16μm,最大粒径D100优选为≤ 50μm;
所述中空二氧化硅的加入量,按质量分数计,更优选为6-15%,中位粒径D50 优选为≥18μm,最大粒径D100优选为≤50μm,堆积密度优选为≤0.5g/cm3,抗压强度优选为≥30MPa,所述中空二氧化硅模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土中位粒径D50优选为≥8μm,最大粒径D100优选为≤30μm;
所述生高岭土的加入量,按质量分数计,优选为0-8%,中位粒径D50为≥ 16μm,最大粒径D100为≤50μm;
所述氧化铝中位粒径D50优选为≥6μm,最大粒径D100优选为≤20μm;
所述片状氢氧化铝的D50优选为1.0-3.0μm。
进一步地,所述有机粘结剂为甲基纤维素,羟丙基纤维素以及甲基纤维素衍生物中的任意一种或其组合;加入量为干混物料质量的1-10%,优选的加入量为干混物料质量的4-7%。
进一步地,所述表面活性剂为硬脂酸、硬脂酸镁、硬脂酸铝、月桂酸及油酸中的任意一种,加入量为干混物料质量的0.5-6%,优选为干混物料质量的1-3%。
进一步地,所述润滑剂为植物油或矿物油中的任意一种,其加入量为干混物料质量的0.5-3%,优选加入量为干混物料质量的1-3%。
进一步地,所述分散剂为水或有机分散剂中的任意一种,所述有机分散剂为乙醇,丙酮中的任意一种,其加入量为干混物料质量的20-35%,优选加入量为 22-28%。
本发明各实施例原料和配比如表2所示,本发明各对比例原料和配比如表3 所示,其中对比例C4堇青石蜂窝陶瓷制品的制备过程中,造孔剂豌豆淀粉是在步骤(1)中随有机粘结剂一起加入无机物料中,并混合均匀,其余制备方法与本发明实施例的制备方法完全相同。
表2各实施例中无机料配比表
表3各对比例中无机料配比表
各实施例和对比例制备的蜂窝陶瓷制品的性能如表4所示:
表4各实施例和对比例制备的蜂窝陶瓷制品的性能
对比例C3,实施例E1-E6是依次增加中空二氧化硅的用量,结果显示随中空二氧化硅的加入量增加产品的孔径和孔隙率增加,但是产品的抗压强度降低。考虑到涂覆性能和产品的强度,作为900目2mil的产品优选的E2-E5,此时中空二氧化硅用量是其加入量为3-21.9%,优选为3-18%,更优选为6-15%。此时所得制品的孔径为5.4-7.9nm,孔隙率为34.1%-38.3%,CTE为0.21-0.35× 10-6/℃,抗压强度为8.1-11.3MPa。烧成合格率≥99.1%。其余的实施例也可以用来制作载体或者是过滤器。
对比例C1是不引入中空二氧化硅的对比例,当不引入中空二氧化硅时产品的孔径是3.0μm,比实施例要小;实施例C2是引入的球形的实心二氧化硅,孔径增加到3.6μm,依旧小于实施例中制品的孔径。这两个对比例和实施例E1-E9 进行对比说明,本发明必须引入中空的二氧化硅。对比例C5-C7与是在实施例 E3的基础上分别替换大中位径的煅烧高岭土、生高岭土和氧化铝为细颗粒的煅烧高岭土、细颗粒的生高岭土和细颗粒的氧化铝。结果显示中值孔径都有所减小,<4μm。去掉煅烧大中位径的煅烧高岭土或者是生高岭土采用大粒径的氧化铝代替,如实施例E7、E8和E9,也可以获得中值粒径在4-10μm的制品。综上所述,中空的二氧化硅加上大粒径的氧化铝或煅烧高岭土、生高岭土形成中值孔径在 4-10μm的制品。对比例C3是之前本公司的发明,使用细颗粒非球形二氧化硅、细颗粒高岭土以及细颗粒氧化铝,制品的孔径很小只有2.9μm,C4是在C3的基础上加入8%的中位粒径在25μm豌豆淀粉,孔径可以增大到4.6μm,但是制品的烧成合格率会降低到76.5%,故不再本发明范围之内。
图2显示本发明实施例E3和E9制品的孔分布相较于对比例C3向大孔径方向移动;实施例E3加入9%的中空二氧化硅以及采用大中位径的煅烧高岭土、生高岭土和氧化铝制备的制品和对比例C4加入8%的淀粉但是采用细颗粒煅烧高岭土、生高岭土和氧化铝所得堇青石制品的孔分布类似。图3显示,对比例C3本公司之前发明采用细颗粒煅烧高岭土、生高岭土和氧化铝所得制品表面的孔较小,实施例E3加入中空二氧化硅以及采用大中位径的煅烧高岭土、生高岭土和氧化铝制品表面孔明显增大与对比例C4加入8%豌豆淀粉造孔剂的结果类似,实施例E9中加入21.9%的中空二氧化硅,产品表面的孔更大。
以上所描述的实施例是本发明一部分实施例,而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
Claims (9)
1.一种薄壁大孔径的堇青石蜂窝陶瓷载体,其特征在于,所述堇青石蜂窝陶瓷载体中堇青石晶相含量>90%,按质量分数计,其化学成分组成为48.0-52.0%的SiO2,33.8-37.4%的Al2O3,13.0-15.5%的MgO,
所述堇青石蜂窝陶瓷载体的中值孔径≥4.3μm,孔隙率≥32.7%,热膨胀系数≤0.35×10-6/℃,A轴抗压≥5.5MPa。
2.根据权利要求1所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体,其特征在于,所述堇青石蜂窝陶瓷载体中堇青石晶相含量≥95%,按质量分数计,其化学成分组成为48.0-52.0%的SiO2,33.8-37.4%的Al2O3,13.0-15.5%的MgO,
所述堇青石蜂窝陶瓷载体的中值孔径≥5.4μm,和/或孔隙率≥34.1%,和/或热膨胀系数≤0.28×10-6/℃,和/或A轴抗压≥8.1MPa。
3.一种如权利要求1所述的薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,包括以下操作步骤:
(1)将无机物料与有机粘结剂干混均匀,得干混物料;无机物料按质量分数计包括41.0-43%滑石、3.0-21.9%中空二氧化硅、13.7-27.8%氧化铝、5.0-19.62%片状氢氧化铝、0-28.3%无机物煅烧高岭土、生高岭土0-14.0%;
(2)在干混物料中加入表面活性剂、润滑剂以及分散剂,湿混,得具有塑性的颗粒;
(3)将塑性的颗粒除去杂质后,在抽真空状态下连续挤出;
(4)将挤出成型后的半成品采用微波处理,同时进行吸风干燥,切割,烧结后,得蜂窝陶瓷载体。
4.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,
所述滑石中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述中空二氧化硅的加入量,按质量分数计,优选为3.0-18.0%,中位粒径D50为≥16μm,最大粒径D100为≤60μm,堆积密度为≤0.6g/cm3,抗压强度为≥20MPa,所述中空二氧化硅由模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土的加入量,按质量分数计,优选为5.9-22.7%,煅烧高岭土中位粒径D50为≥6μm,最大粒径D100为≤35μm;
所述生高岭土的加入量,按质量分数计,优选为0-8.0%,中位粒径D50为≥14μm,最大粒径D100为≤60μm;
所述氧化铝的加入量,按质量分数计,优选为16.2-23.9%,中位粒径D50为≥4μm,最大粒径D100为≤25μm;
所述片状氢氧化铝的加入量,按质量分数计,优选为5.0-10.0%,D50为0.2-4.0μm,所述片状氢氧化铝采用水解铝法制得,具体操作为:采用液氮急速冷却的方法,在106-107K/S的极冷过程中,金属铝表面会产生大量的空位,错位及层错的缺陷,增加金属铝的活性,与水反应后,产生片状,高活性,高纯度,高表面积氢氧化铝,成品中钾、钠元素的总质量含量低于0.1%。
5.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,
所述滑石中位粒径D50优选为≥16μm,最大粒径D100优选为≤50μm;
所述中空二氧化硅的加入量,按质量分数计,更优选为6-15%,中位粒径D50优选为≥18μm,最大粒径D100优选为≤50μm,堆积密度优选为≤0.5g/cm3,抗压强度优选为≥30MPa,所述中空二氧化硅模板法、喷雾干燥法、微乳液法中的任意一种方法制成;
所述煅烧高岭土中位粒径D50优选为≥8μm,最大粒径D100优选为≤30μm;
所述生高岭土的加入量,按质量分数计,优选为0-8%,中位粒径D50为≥16μm,最大粒径D100为≤50μm;
所述氧化铝中位粒径D50优选为≥6μm,最大粒径D100优选为≤20μm;
所述片状氢氧化铝的D50优选为1.0-3.0μm。
6.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,所述有机粘结剂为甲基纤维素,羟丙基纤维素以及甲基纤维素衍生物中的任意一种或其组合;加入量为干混物料质量的1-10%,优选的加入量为干混物料质量的4-7%。
7.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,所述表面活性剂为硬脂酸、硬脂酸镁、硬脂酸铝、月桂酸及油酸中的任意一种,加入量为干混物料质量的0.5-6%,优选为干混物料质量的1-3%。
8.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,所述润滑剂为植物油或矿物油中的任意一种,其加入量为干混物料质量的0.5-3%,优选加入量为干混物料质量的1-3%。
9.根据权利要求3所述的一种薄壁大孔径的堇青石蜂窝陶瓷载体的制备方法,其特征在于,所述分散剂为水或有机分散剂中的任意一种,所述有机分散剂为乙醇,丙酮中的任意一种,其加入量为干混物料质量的20-35%,优选加入量为22-28%。
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