CN111087252A - 高强度多孔陶瓷过滤器及其制备方法 - Google Patents

高强度多孔陶瓷过滤器及其制备方法 Download PDF

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CN111087252A
CN111087252A CN201911257626.XA CN201911257626A CN111087252A CN 111087252 A CN111087252 A CN 111087252A CN 201911257626 A CN201911257626 A CN 201911257626A CN 111087252 A CN111087252 A CN 111087252A
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porous ceramic
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王安英
李世慧
张金钊
孟姗姗
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Shandong Sicer Novel Material Co ltd
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Abstract

本发明属于陶瓷材料技术领域，具体涉及一种高强度多孔陶瓷过滤器及其制备方法。所述的高强度多孔陶瓷过滤器，陶瓷材料组分包括50‑90wt％的氧化锆和10‑50wt％的产物D；所述产物D的制备方法为：(1)以活性氢氧化铝为原料进行低温煅烧后得到产物A；(2)产物A与纳米α‑氧化铝、硅溶胶、金属盐混合，加水球磨混合得产物B；(3)混合产物B经过烘干、煅烧得到产物C，产物C经过蒸馏水清洗后，烘干得到粉体混合产物D。本发明的高强度多孔陶瓷过滤器，在常温、高温强度都有明显提升，抗金属冲击能力提高，同时成本明显降低，适合工业化生产；本发明还提供其制备方法。

Description

高强度多孔陶瓷过滤器及其制备方法
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种高强度多孔陶瓷过滤器及其制备方法。
背景技术
泡沫陶瓷过滤器是一种气孔率高达70～90％的具有三维立体网络骨架和相互贯通气孔结构的多孔陶瓷制品，由于其具有耐高温、耐腐蚀、气孔率高、比表面积大、密度小、对流体自扰性强等特点，所以广泛应用于耐高温环境下的流体过滤净化、催化剂载体等领域。其用于金属液过滤净化，可高效率的去除金属液中大块的夹杂物和大部分小至微米的微小悬浮夹杂物，并促进部分气体的析出，从而大大降低铸件废品率，提高铸件质量和成品率，降低生产成本提高生产效率。在铸钢时，由于钢液的温度高达1600℃以上，其使用的泡沫陶瓷过滤器目前普遍采用氧化镁稳定氧化锆来制备。
专利CN200710115193.5公开了一种氧化锆材质泡沫陶瓷的制备方法，主要以氧化锆添加少量或部分稳定剂为原料来制备氧化锆材质泡沫陶瓷过滤器，其优势是为了降低成本采用了单晶氧化锆。通过加入稳定剂及少量添加剂制备氧化锆泡沫陶瓷是目前普遍的方式，但是制备的氧化锆泡沫陶瓷往往由于高温晶型转变导致力学性能衰减，抗侵蚀能力也将低，导致在一些高温下需要长期使用的场合，产品往往失效。
专利CN200710139288.0公布了一种氧化锆泡沫陶瓷过滤器，其中引入了10～15％的氧化铝，但是由于根据对氧化锆材质泡沫陶瓷过滤器的要求，用作陶瓷粉末的粒度采用大于320目，且引入的氧化铝含量不高，更多的是起到降低成本的作用，对于稳定氧化锆晶型，提高产品强度尤其是高温性能作用不大。
专利CN1662286A、CN201510436071.0都公开了用纤维增强泡沫陶瓷的方法，尤其是专利CN201510436071.0公开了一种用氧化锆短纤维增强氧化锆泡沫陶瓷的方法，一定程度上提高了氧化锆泡沫陶瓷的高温性能，但是氧化锆纤维价格昂贵，而且不容易分散。上述泡沫陶瓷过滤器的研究虽然取得了一定的成果，但是仍然存在高温不稳定、耐高温侵蚀性能欠佳，成本较高等问题。
发明内容
针对现有技术的不足，本发明的目的是提供一种高强度多孔陶瓷过滤器，在常温、高温强度都有明显提升，抗金属冲击能力提高，同时成本明显降低，适合工业化生产；本发明还提供其制备方法。
本发明所述的高强度多孔陶瓷过滤器，陶瓷材料组分包括50-90wt％的氧化锆和10-50wt％的产物D；
所述产物D的制备方法为：
(1)以活性氢氧化铝为原料进行低温煅烧后得到产物A；
(2)产物A与纳米α-氧化铝、硅溶胶、金属盐混合，加水球磨混合得产物B；
(3)混合产物B经过烘干、煅烧得到产物C，产物C经过蒸馏水清洗后，烘干得到粉体产物D。
步骤(1)中煅烧温度为300～600℃，煅烧时间1～3h。
步骤(2)中纳米α-氧化铝的质量为产物A质量的5～20％；产物A和纳米α-氧化铝的质量之和为金属盐质量的25～50％；硅溶胶中氧化硅的质量为产物A和纳米α-氧化铝质量之和的0.1～5％。
步骤(2)中金属盐为NaCl、KCl、Na2SO4、K2SO4中的一种或多种。
步骤(2)中球磨所用球石为氧化铝球石，料球比1:1～2；球磨水含量30～50％。
步骤(3)中混合物B的烘干温度为50～100℃，煅烧温度为700～1000℃，煅烧时间为1～4h。
以活性氢氧化铝为主要原料制备的粉体产物D为高长径比粉体和高径厚比粉体的混合物，其中高长径比粉体的长径比达10-200，高径厚比粉体的径厚比可达10-100，产物D的粉体表面光滑平整，比表面大，独特的片状结构和线状结构在浆料中具有很好的分散和悬浮效果，烧成后形成搭桥和咬合结构，能够明显增强多孔陶瓷体的强度，而且产物D的加入可以抑制氧化锆的高温相变，提高陶瓷体的高温强度和性能。
本发明所述的高强度多孔陶瓷过滤器的制备方法，步骤如下：
将产物D与氧化锆骨料混合，加入水、胶、添加剂、分散剂快速搅拌得到浆料，浆料陈腐后，将一定形状的聚氨酯泡沫浸渍于浆料中，并用辊压机挤出多余浆料，使浆料均匀涂覆于聚氨酯海绵上，干燥后，经高温烧结，得到多孔陶瓷过滤器。
以质量百分比计，浆料的各原料组成如下：
Figure BDA0002310731070000021
氧化锆为单斜氧化锆，粒度D50＝10～30μm。
胶为PVA、CMC、黄原胶、阿拉伯树胶中的一种或多种。
添加剂为氧化镁、氧化钙、氧化钇、氧化镧、氧化铈中的一种或多种；优选为氧化钙。
分散剂为柠檬酸钠。
陈腐时间为4～48h，干燥温度为25～100℃，高温烧结温度为1500～1600℃，高温烧结保温时间为2～5h。
与现有技术相比，本发明具有以下有益效果：
(1)本发明在氧化锆中引入以活性氢氧化铝为主要原料制备的产物D，大大降低了产品成本，且高径厚比粉体和高长径比粉体混合的产物D易于分散，效果及原理可等同于晶须，并抑制了氧化锆的高温相变，有效增强了多孔陶瓷体的常温和高温强度，降低了高温强度衰减，抗金属溶液冲击能力提高；
(2)本发明的制备方法简单，工艺条件易于控制，便于工厂大规模生产。
具体实施方式
以下结合实施例对本发明做进一步说明，但本发明的保护范围不仅限于此，该领域专业人员对本发明技术方案所作的改变，均应属于本发明的保护范围内。
所述方法如无特别说明均为常规方法，所述原材料如无特别说明均能从公开商业途径而得。
实施例1
按以下方法制备产物D：
(1)将活性氢氧化铝在500℃温度下煅烧2h，得到产物A；
(2)将500g产物A与30g纳米α-氧化铝、50g固含量30％的硅溶胶、800g氯化钠、500g水混合，采用氧化铝球石，料球比1:1.5，球磨2h，得到混合产物B；
(3)混合产物B经过120℃烘干、900℃电炉煅烧3h，冷却后得到产物C，产物C用蒸馏水清洗后，100℃烘干得到粉体产物D。
实施例2-4和对比例1-4
按照表1的原料配方制备浆料，浆料陈腐后，分别涂覆在75mm×75mm×25mm，孔径10PPI的聚氨酯泡沫上，制备的泡沫陶瓷坯体室温干燥后，按照表1的烧结温度进行烧成，保温2h，得到多孔陶瓷过滤器。
对实施例1-3和对比例1-4制备的多孔陶瓷过滤器进行性能测试，测试方法为50mm三点抗折压力，测试结果如表1所示。
表1 实施例2-4和对比例1-2的浆料配方、烧成温度、产品性能指标
Figure BDA0002310731070000041
从表1可以看出，本发明制备的多孔陶瓷过滤器的常温强度有明显的提高，同时抗热震性能提升，高温强度衰减也降低，耐高温金属溶液的侵蚀和冲击性能明显提升，同时成本降低，更具有经济价值。对比例1与实施例相比，将产物D替换为普通刚玉粉，对比例2与实施例相比，不含产物D和刚玉粉，其制备的多孔陶瓷过滤器常温强度均低于实施例，高温强度衰减较大，且高含量氧化锆的使用导致产品成本较高。对比例3与实施例相比，产物D的含量较低，对比例4与实施例相比，产物D的含量较高，从测试结果可以看到，当产物的用量过低或过高时，其制备的多孔陶瓷过滤器的各项性能均无法达到较佳的效果，耐钢水侵蚀性能较差。

Claims (10)

1.一种高强度多孔陶瓷过滤器，其特征在于：陶瓷材料组分包括50-90wt％的氧化锆和10-50wt％的产物D；
所述产物D的制备方法为：
(1)以活性氢氧化铝为原料进行低温煅烧后得到产物A；
(2)产物A与纳米α-氧化铝、硅溶胶、金属盐混合，加水球磨混合得产物B；
(3)混合产物B经过烘干、煅烧得到产物C，产物C经过蒸馏水清洗后，烘干得到粉体产物D。
2.根据权利要求1所述的高强度多孔陶瓷过滤器，其特征在于：步骤(1)中煅烧温度为300～600℃，煅烧时间1～3h。
3.根据权利要求1所述的高强度多孔陶瓷过滤器，其特征在于：步骤(2)中纳米α-氧化铝的质量为产物A质量的5～20％；产物A和纳米α-氧化铝的质量之和为金属盐质量的25～50％；硅溶胶中氧化硅的质量为产物A和纳米α-氧化铝质量之和的0.1～5％。
4.根据权利要求1所述的高强度多孔陶瓷过滤器，其特征在于：步骤(2)中金属盐为NaCl、KCl、Na2SO4、K2SO4中的一种或多种。
5.根据权利要求1所述的高强度多孔陶瓷过滤器，其特征在于：步骤(2)中球磨所用球石为氧化铝球石，料球比1:1～2；球磨水含量30～50％。
6.根据权利要求1所述的高强度多孔陶瓷过滤器，其特征在于：步骤(3)中混合物B的烘干温度为50～100℃，煅烧温度为700～1000℃，煅烧时间为1～4h。
7.根据权利要求1-6任一项所述的高强度多孔陶瓷过滤器的制备方法，其特征在于：步骤如下：
将产物D与氧化锆骨料混合，加入水、胶、添加剂、分散剂快速搅拌得到浆料，浆料陈腐后，将一定形状的聚氨酯泡沫浸渍于浆料中，并用辊压机挤出多余浆料，使浆料均匀涂覆于聚氨酯海绵上，干燥后，经高温烧结，得到多孔陶瓷过滤器。
8.根据权利要求7所述的高强度多孔陶瓷过滤器的制备方法，其特征在于：以质量百分比计，浆料的各原料组成如下：
Figure FDA0002310731060000011
Figure FDA0002310731060000021
9.根据权利要求7所述的高强度多孔陶瓷过滤器的制备方法，其特征在于：氧化锆为单斜氧化锆，粒度D50＝10～30μm；
胶为PVA、CMC、黄原胶、阿拉伯树胶中的一种或多种；
添加剂为氧化镁、氧化钙、氧化钇、氧化镧、氧化铈中的一种或多种；
分散剂为柠檬酸钠。
10.根据权利要求7所述的高强度多孔陶瓷过滤器的制备方法，其特征在于：步骤(4)中陈腐时间为4～48h，干燥温度为25～100℃，高温烧结温度为1500～1600℃，高温烧结保温时间为2～5h。
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