CN108249904B - 一种吸水率稳定的蜂窝陶瓷载体及其制备方法 - Google Patents

一种吸水率稳定的蜂窝陶瓷载体及其制备方法 Download PDF

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CN108249904B
CN108249904B CN201810048730.7A CN201810048730A CN108249904B CN 108249904 B CN108249904 B CN 108249904B CN 201810048730 A CN201810048730 A CN 201810048730A CN 108249904 B CN108249904 B CN 108249904B
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李军虎
张金龙
田建刚
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JINCHENG FUJI NEW MATERIAL CO Ltd
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Abstract

本发明公开了一种吸水率稳定的蜂窝陶瓷载体及其制备方法，以滑石、氧化铝、高岭土、无定形石英以及氢氧化铝微粉组成陶瓷前驱体粉末，通过控制每种原材料的松装密度及粒径分布，再加入粘结剂、润滑剂、保水剂，制备可塑性泥料，通过筛料、高速混料、调泥、真空练泥、成型、烘干、高温烧结制成蜂窝陶瓷载体，本发明方法制备的蜂窝陶瓷过滤器吸水率稳定、机械强度高、热震稳定性好，而且具有成本低、操作简单，适应于工业化生产的优点。

Description

一种吸水率稳定的蜂窝陶瓷载体及其制备方法
技术领域
本发明涉及蜂窝陶瓷载体技术领域，具体地说，涉及一种吸水率稳定的蜂窝陶瓷载体及其制备方法。
背景技术
目前，国内已强制执行国Ⅴ标准，部分地区已执行国Ⅵ标准。因此要求汽车发动机厂家在尾气排放前对尾气进行催化处理。而催化处理的关键部件堇青石蜂窝陶瓷载体的质量稳定性会影响到催化剂的质量。堇青石蜂窝陶瓷载体是汽油车、柴油车催化剂、DOC、SCR等催化剂的主要载体，其主要功能是提供有效的表面和适宜的孔结构，维持催化剂活性相性组分高度分散；增强催化剂的机械强度，使催化剂具有一定的形状和大小；改善催化剂的热传导性能，以满足反应过程的传热要求和减少活性组分的用量。
蜂窝陶瓷载体的关键指标：抗热震性会影响到催化剂的使用寿命；吸水率的稳定会影响催化剂使用的稳定性，防止催化剂脱落影响尾气处理效率。
目前，现有技术中主要是在提高蜂窝陶瓷热震性方面和提高载体成活率方面。专利201310450481.1提到了大规格堇青石蜂窝陶瓷载体的制备方法，主要是针对原材料进行改性，从而提高载体的成活率，降低生产成本。专利201610141755.2针对原位合成堇青石的原料物料的物理、化学特性的不同对平均粒径进行调整，使合成的堇青石物料具有较高放入致密性，这样在挤出成型过程中蜂窝陶湿坯有较高的强度，从而减少缺陷。专利200680018821.1是提供足够的强度与超低的热膨胀性相结合的改良型堇青石陶瓷及其制备方法，热膨胀系数≤-0.6x10-7/℃。
现有技术中都是针对蜂窝陶瓷载体的机械性能、抗震度、强度以及提高载体的成活率来对蜂窝陶瓷载体进行改进，都忽视了蜂窝陶瓷载体的另一影响蜂窝陶瓷载体性能的关键指标吸水率。
有鉴于此，如何提供一种通过控制蜂窝陶瓷载体吸水率来进一步提高蜂窝陶瓷载体的性能。
发明内容
有鉴于此，本发明提供了一种吸水率稳定的蜂窝陶瓷载体及其制备方法，通过控制蜂窝陶瓷载体的吸水率来提高陶瓷过滤器吸水率稳定性，大大提高了催化剂防脱性能，提高了尾气处理效率。
为了实现上述目的，本发明采用如下技术方案：
一种吸水率稳定的蜂窝陶瓷载体，包括前躯体粉末与助剂，所述前躯体粉末与所述助剂重量配比为85～90:10～15；
所述前躯体粉末由下述重量配比的原料构成：
Figure GDA0001588609750000021
所述助剂由下述重量配比的原料构成：
Figure GDA0001588609750000022
Figure GDA0001588609750000031
优选地，所述前躯体粉末由下述重量配比的原料构成：
Figure GDA0001588609750000032
所述助剂由下述重量配比的原料构成：
Figure GDA0001588609750000033
一种吸水率稳定的蜂窝陶瓷载体的制备方法，包括如下步骤：
1)按照上述的一种吸水率稳定的蜂窝陶瓷载体的配方称取各原料，然后将滑石、超细ɑ～氧化铝微粉、高岭土、无定形石英以及氢氧化铝微粉原材料筛分，随后添加羟丙基甲基纤维素、硬脂酸盐，高速混合，混合后松装密度为0.4～0.6g/cm3；
2)在所述步骤1)制备好混合物中继续添加甘油、润滑油、纯水，然后进行捏合，真空练泥，陈腐，再挤出成型；
3)将所述步骤2)中成型后的坯体进行微波干燥、切割、烧成，烧成温度为1400～1420℃，然后进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，同时在保温过程中进行取样，实时测定载体在炉内的吸水率控制在23±0.2％，保温时间为10小时，即制得蜂窝陶瓷载体。
优选地，所述步骤2)中真空度为0.7～0.95。
优选地，所述步骤1)中滑石的松装密度为0.4～0.5g/cm3,粒径D50＝10～14μm，K2O+Na2O+CaO含量≤0.5％。
优选地，所述步骤1)中超细ɑ-氧化铝微粉的松装密度为0.7～0.8g/cm3,粒径D50＝1～2μm，K2O+Na2O含量≤0.1％。
优选地，所述步骤1)中高岭土的松装密度为0.22～0.3g/cm3,粒径D50＝1～4μm，K2O+Na2O+CaO含量≤0.4％。
优选地，所述步骤1)中无定形石英的松装密度为0.4～0.5g/cm3,粒径D50＝3～5μm，K2O+Na2O含量≤0.1％。
优选地，所述步骤1)中氢氧化铝微粉的松装密度为0.15～0.25g/cm3,粒径D50＝1～2.5μm，K2O+Na2O含量≤0.3％。
本发明的有益效果：
1)本发明通过对原材料松装密度，粒径，练泥过程，烧成过程的精细控制，对每道影响载体吸水率的生产工序都提出可调整的要求，特别是在烧成保温时对炉内不同位置点温度控制在5℃以内，对载体进行实时控制，使其载体吸水率控制在23±0.2％,从而可保证出厂产品吸水率保持在22～24％；
2)本发明通过调整真空练泥机真空度(0.7～0.95)改变泥料致密度，从而改变载体的吸水率；
3)通过本发明生产的产品，性能指标为：热膨胀系数≤1.2*10-6，抗热震性(0～650℃)空冷3次不开裂，吸水率22～24％，抗压强度≥15MPa。
具体实施方式
下面将结合本发明的实施例，对本发明的技术方案进行完整、清楚的描述。
以下各实施例中所述的前躯体粉末包括：滑石，超细ɑ～氧化铝微粉，高岭土，无定形石英，氢氧化铝微粉；助剂包括：羟丙基甲基纤维素，硬脂酸盐，甘油，润滑油，纯水。
实施例1
本发明中该吸水率稳定的蜂窝陶瓷载体的制备方法，包括如下步骤：
1)按滑石35份，超细ɑ-氧化铝微粉10份，高岭土10份，无定形石英5份，氢氧化铝微粉3份，羟丙基甲基纤维素2份，硬脂酸盐1份，甘油2份，润滑油0.5份，纯水25份配方称取各原料，，然后将滑石、超细ɑ～氧化铝微粉、高岭土、无定形石英以及氢氧化铝微粉原材料筛分，随后添加羟丙基甲基纤维素、硬脂酸盐，前躯体粉末与所述助剂重量配比为85:10，高速混合，混合后松装密度为0.54g/cm3；
2)在所述步骤1)制备好混合物中继续添加甘油、润滑油、纯水，然后进行捏合，真空练泥，真空度为0.7，陈腐，再挤出成型；
3)将所述步骤2)中成型后的坯体进行微波干燥、切割、烧成，烧成温度为1400℃，然后进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，同时在保温过程中进行取样，实时测定载体在炉内的吸水率控制在23±0.2％，保温时间为10小时，即制得蜂窝陶瓷载体。
其中，步骤1)中滑石的松装密度为0.42g/cm3,粒径D50＝10μm，K2O+Na2O+CaO含量≤0.5％；超细ɑ-氧化铝微粉的松装密度为0.92g/cm3,粒径D50＝1μm，K2O+Na2O含量≤0.1％；高岭土的松装密度为0.28g/cm3,粒径D50＝1μm，K2O+Na2O+Ca0含量≤0.4％；无定形石英的松装密度为0.5g/cm3,粒径D50＝3μm，K2O+Na2O含量≤0.1％；氢氧化铝微粉的松装密度为0.18g/cm3,粒径D50＝1μm，K2O+Na2O含量≤0.3％。
实施例2-4采用如实施例1中制备蜂窝陶瓷载体的制备工艺，仅是改变前躯体粉末以及混合原料的松装密度，然后检测实施例1-4的吸水率，具体参数参见表1：
表1
Figure GDA0001588609750000061
从表1中可以看出，通过调节前躯体粉末的松装密度可以进一步改善制备的蜂窝陶瓷载体的吸水率。
实施例5-7参见实施例1的制备工艺，改变实施例5-7中每个实施例中的真空度，检测每个实施例制备的蜂窝陶瓷载体的吸水率，具体参数参见表2：
表2
Figure GDA0001588609750000062
Figure GDA0001588609750000071
通过表2可以看出，通过调整真空练泥机真空度(0.7～0.95)改变泥料致密度，从而改变载体的吸水率。
实施例8-11参见实施例1的制备工艺，改变实施例8-11中每个实施例中步骤3)的烧成温度，检测每个实施例制备的蜂窝陶瓷载体的吸水率，具体参数参见表3：
表3
实施例 烧成温度 吸水率
实施例8 1415 21.9
实施例9 1405 22.8
实施例10 1395 23.6
实施例11 1385 24.5
通过表3可以看出，通过调节步骤3中烧成温度，同样可以控制蜂窝陶瓷载体的吸水率。
通过上述实施例1-11可以得出，前躯体粉末的松装密度、真空度以及烧成温度均是影响蜂窝陶瓷载体吸水率的重要因素，同时对于本发明实施例中未提及的前躯体粉末的粒径、原料的配比也是影响蜂窝陶瓷载体吸水率重要因素，通过调节原料的配比、前躯体粉末的松装密度、前躯体粉末的粒径、真空度以及烧成温度来进一步使蜂窝陶瓷载体吸水率保持在22～24％；而上述影响吸水率的因素众多，所以，有限次的试验或正交试验并无法获得本发明的技术方案，而吸水率在22～24％的蜂窝陶瓷载体提高了催化剂使用的稳定性，防止催化剂脱落，提高了尾气处理效率；
实施例12
一种吸水率稳定的蜂窝陶瓷载体及其制备方法，它由前躯体粉末和助剂构成。粉料及助剂比例见表4：
Figure GDA0001588609750000081
1)取松装密度为0.42g/cm3,粒径D50＝12.2μm的滑石，松装密度为0.72g/cm3,粒径D50＝1.2μm的超细ɑ-氧化铝微粉，松装密度为0.23g/cm3,粒径D50＝2μm的片状高岭土，松装密度为0.42g/cm3,粒径D50＝3.7μm.的无定形石英，松装密度为0.22g/cm3,粒径D50＝1.2μm的氢氧化铝微粉，分别通过孔径为0.10mm的筛网，随后添加硬脂酸盐、羟丙基甲基纤维素，按表1所述比例进行配料，高速混合，混合后松装密度为0.43g/cm3；
2)将高速混合的粉料添加甘油、润滑油、纯水进行捏合、真空练泥(真空度0.9)，陈腐，挤出成型；
3)将成型后的坯体进行微波干燥、切割、烧成，保温时间10小时；同时在保温过程中进行生产取样，保证取样载体吸水率保持在23±0.2％之间，根据取样载体吸水率确定烧成温度为1410℃，出炉产品吸水率范围为22.5～23.5。
通过对本实施例生产的产品，采用GB/T 25949-2010蜂窝陶瓷国家标准对产品进行性能测试，测试性能指标为：热膨胀系数1.0*10-6，抗热震性(0～650℃)空冷3次不开裂，吸水率22.5～23.5％，抗压强度≥15MPa。
实施例13
1)取松装密度为0.48g/cm3,粒径D50＝13.5μm的滑石，松装密度为0.78g/cm3,粒径D50＝1.8μm的超细ɑ-氧化铝微粉，松装密度为0.29g/cm3,粒径D50＝3.5μm的片状高岭土，松装密度为0.45g/cm3,粒径D50＝4.2μm.的熔融石英，松装密度为0.24g/cm3,粒径D50＝1.7μm的氢氧化铝微粉，分别通过孔径为0.10mm的筛网，随后添加硬脂酸盐、羟丙基甲基纤维素.按表1所述比例进行配料，高速混合，混合后松装密度为0.55g/cm3，
2)将高速混合的粉料添加甘油、润滑油、纯水进行捏合、真空练泥(真空度0.95(由于载体松装密度偏上限，会导致产品吸水率偏大，需提高真空度，方可控制吸水率)，陈腐，挤出成型
3)将成型后的坯体进行微波干燥、切割、烧成，保温时间10小时。同时在保温过程中进行生产取样，保证取样载体吸水率保持在23±0.2％之间，根据取样载体吸水率确定烧成温度为1415℃(由于载体松装密度偏上限，导致吸水率偏大，需提高温度，方可控制吸水率)，出炉产品吸水率范围为22.5～23.5。
4)通过本实施例生产的产品，采用GB/T 25949-2010蜂窝陶瓷国家标准对产品进行性能测试，测试性能指标为：热膨胀系数1.1*10-6，抗热震性(0～650℃)空冷3次不开裂，吸水率22.8～23.5％，抗压强度≥15MPa。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (2)

1.一种吸水率稳定的蜂窝陶瓷载体，其特征在于，包括前躯体粉末与助剂，所述前躯体粉末与所述助剂重量配比为85～90:10～15；
所述前躯体粉末由下述重量配比的原料构成：
Figure FDA0003022410990000011
所述助剂由下述重量配比的原料构成：
Figure FDA0003022410990000012
其制备方法包括以下步骤：
1)按照上述的一种吸水率稳定的蜂窝陶瓷载体的配方称取各原料，然后将滑石、超细ɑ～氧化铝微粉、高岭土、无定形石英以及氢氧化铝微粉原材料筛分，随后添加羟丙基甲基纤维素、硬脂酸盐，高速混合，混合后松装密度为0.4～0.6g/cm3；
2)在所述步骤1)制备好混合物中继续添加甘油、润滑油、纯水，然后进行捏合，真空练泥，陈腐，再挤出成型；
3)将所述步骤2)中成型后的坯体进行微波干燥、切割、烧成，烧成温度为1400～1420℃，然后进行保温，保温过程中，对每个测温点进行实时测温，单独调整，保证炉内不同位置温度控制在0～5℃以内，同时在保温过程中进行取样，实时测定载体在炉内的吸水率控制在23±0.2％，保温时间为10小时，即制得蜂窝陶瓷载体；
所述步骤1)中滑石的松装密度为0.4～0.5g/cm3,粒径D50＝10～14μm，K2O+Na20+Ca0含量≤0.5％；
所述步骤1)中超细ɑ-氧化铝微粉的松装密度为0.7～0.8g/cm3,粒径D50＝1～2μm，K2O+Na2O含量≤0.1％；
所述步骤1)中高岭土的松装密度为0.22～0.3g/cm3,粒径D50＝1～4μm，K2O+Na2O+Ca0含量≤0.4％；
所述步骤1)中无定形石英的松装密度为0.4～0.5g/cm3,粒径D50＝3～5μm，K2O+Na2O含量≤0.1％；
步骤1)中氢氧化铝微粉的松装密度为0.15～0.25g/cm3,粒径D50＝1～2.5μm，K2O+Na2O含量≤0.3％；
所述步骤2)中真空度为0.7～0.95Mpa。
2.根据权利要求1所述的一种吸水率稳定的蜂窝陶瓷载体，其特征在于，
Figure FDA0003022410990000031
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