CN110256063B - 一种莫来石/白榴石多孔陶瓷复合材料的制备方法 - Google Patents

一种莫来石/白榴石多孔陶瓷复合材料的制备方法 Download PDF

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CN110256063B
CN110256063B CN201910670218.0A CN201910670218A CN110256063B CN 110256063 B CN110256063 B CN 110256063B CN 201910670218 A CN201910670218 A CN 201910670218A CN 110256063 B CN110256063 B CN 110256063B
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闫姝
章凡勇
李大纲
都兴红
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Northeastern University China
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Abstract

本发明公开了一种莫来石/白榴石多孔陶瓷复合材料的制备方法，利用可发泡的含漂珠/无机聚合物复合材料为前驱体，双氧水和漂珠在室温复合造孔方式，结合高温处理获得轻质多孔莫来石/白榴石陶瓷复合材料。本发明的制备过程为：1.无机聚合物激发溶液的制备；2.可发泡的含漂珠/无机聚合物复合浆料配置；3.固化；4.陶瓷转化。室温的发泡丰富了无机聚合物材料的三维网络结构，漂珠的加入丰富了其多级孔构成，克服了高强度高孔隙率三维多孔陶瓷复合材料制备困难的问题，实现了高强高孔隙率多孔陶瓷复合材料的大块低成本的制备，该材料可用于防火保温，吸附过滤，环境保护等领域。制备方法原料成本低廉，成型工艺简单，绿色环保，适于大规模生产。

Description

一种莫来石/白榴石多孔陶瓷复合材料的制备方法
技术领域
本发明属于多孔陶瓷复合材料制备领域，涉及一种莫来石/白榴石多孔陶瓷复合材料的制备方法，尤其涉及到一种漂珠/泡沫无机聚合物复合材料为前驱体转化的多孔陶瓷基复合材料的制备方法。
背景技术
众所周知，多孔陶瓷具有多孔结构，良好耐高温和化学稳定性等优点，在工业、化工、冶金等领域具有广阔的应用前景。开孔结构的多孔陶瓷在过滤分离、污水处理等领域有较好的应用，闭孔结构的多孔陶瓷在保温隔热、防火等领域也具有大的应用空间。常用的传统制备工艺主要有颗粒堆积、添加造孔剂、直接发泡和溶胶-凝胶等方法。随着时代的发展，陶瓷基复合材料展现出了一定优势，在制备方面，前驱体转化法被视作一种有效的方法，通过前驱体高温转化，可以获得具有纳米组织的陶瓷，组织均匀，性能优良。无机聚合物材料是一种低温制备的以硅铝氧为主的材料，不同的硅铝比成分又决定着其不同的结构。此外，近年来的研究表明，无机聚合物也可视作一种新型绿色前驱体，通过适当的高温处理可以获得特定组成与结构的陶瓷材料，机械性能同样良好。
而在多孔陶瓷制备的过程中，孔隙率和强度的变化存在相互制约的关系，提高孔隙率的同时，如何使其强度仍达到工程需要，则是需要解决的问题。漂珠是从粉煤灰中提取出的一种中空微球，它是电厂的副产物，对漂珠的再利用逐渐受到人们的重视。利用其特殊的中空结构，可以将其作为造孔剂制备多孔材料。
发明内容
本发明针对高孔隙率轻质高强多孔陶瓷的低成本绿色制备问题，提供了一种莫来石/白榴石多孔陶瓷复合材料的制备方法。利用可发泡的含漂珠/无机聚合物复合材料为前驱体的转化法，通过双氧水和漂复合造孔，结合后续高温处理，获得轻质莫来石/白榴石多孔陶瓷复合材料，陶瓷复合材料的制备工艺绿色无污染，工艺简单、操作便捷、适用范围广泛。获得的多孔陶瓷复合材料强度高，质量轻、孔隙可控，在建筑、保温、吸附、过滤等领域有应用潜能。本发明制备了一种莫来石/白榴石多孔陶瓷复合材料，提供了一莫来石/白榴石多孔陶瓷复合材料的制备方法，解决了上述问题。
本发明解决技术问题，采用如下技术方案：
本发明利用无机聚合物可作为陶瓷前驱体应用的特性，利用可发泡的含漂珠/无机聚合物复合材料为前驱体，结合发泡剂原位发泡与漂珠造孔二者优势结合，获得了轻质高强且孔隙可控的莫来石/白榴石多孔陶瓷复合材料，其特点在于：以活性矿物粉体、漂珠、碱激发溶液等为原料，结合发泡剂和漂珠协同造孔及无机聚合物可陶瓷化的特性优势，将室温漂珠/泡沫无机聚合物三维多孔结构直接转化为莫来石/白榴石多孔陶瓷复合材料。制备过程按照如下步骤进行：
步骤一、无机聚合物碱激发溶液的制备：将质量分数30-40％的硅溶胶与氢氧化钾按照摩尔比为1:1.5～3混合并磁力混合3-7天至混合均匀，得到无机聚合物碱激发溶液；
步骤二、可发泡的含漂珠/无机聚合物复合浆料配置：将活性矿物粉体加入步骤一所得的无机聚合物碱激发溶液中，满足其中硅铝比为2，加入去离子水调节料浆粘度为100mPa·s～500mPa·s之间，搅拌充分20-50分钟，获得硅铝比为2的无机聚合物浆料，再在其中加入漂珠，漂珠与矿物粉体质量比1-5:1，继续搅拌20-50分钟，加入双氧水和十二烷基硫酸钠，其中双氧水与活性矿物粉体质量比为1％-20％，十二烷基硫酸钠与活性矿物粉体质量比为0-10％，继续搅拌10分钟，获得可发泡的含漂珠/无机聚合物复合浆料；
步骤三、漂珠/泡沫无机聚合物复合材料的固化：将步骤三得到的混合浆料倒入模具中，置于15-35℃温度下静置6-24小时发泡，再将发泡的复合材料置于40-60℃温度下静置24-120小时固化，脱模后获得漂珠/泡沫无机聚合物复合材料。
步骤四、莫来石/白榴石多孔陶瓷复合材料陶瓷转化：在空气或保护气氛下，对步骤三获得的漂珠/泡沫无机聚合物复合材料高温处理，升温速度1℃/min～5℃/min，升温至900-1300℃，保温2-5小时后降温，降温速度5℃/min～10℃/min冷却至室温，取出后获得莫来石/白榴石多孔陶瓷复合材料。
进一步地，上述所述的活性矿物粉体为偏高岭土。
进一步地，上述步骤四中优选升温至1000-1200℃。
与已有技术相比，本发明的优异效果体现在：
本发明在无机聚合物材料可作为陶瓷前驱体使用的基础上，采用在无机聚合物制备过程中将漂珠与其复合，将可发泡的含漂珠/无机聚合物复合材料视作前驱体，结合双氧水与漂珠二者共同结合的方式造孔，在室温对漂珠/无机聚合物复合材料发泡，固化具有三维网状的获得漂珠/泡沫无机聚合物复合材料，对其进行一定的高温处理，获得了高强高孔隙率的多孔陶瓷复合材料。双氧水的发泡可使无机聚合物材料具有三维网状大孔结构。漂珠的成分与基体无机聚合物元素组成接近，有良好的相容性，可实现与无机聚合物基体的有效结合，漂珠作为造孔剂的加入，直接对基体造孔，保留了其丰富完整的微米尺度的孔隙结构。对固化的复合材料经过适当的高温处理，即可获得莫来石/白榴石多孔陶瓷复合材料，工艺简单，便捷，孔隙可控。本发明涉及漂珠/无机聚合物复合材料的发泡、固化，以及莫来石/白榴石多孔陶瓷复合材料的高温陶瓷化转变。获得的多孔复合材料具有质量轻、强度高、孔隙率高等特点，且成型工艺简单、可操作性强、适合复杂构件的制备及大尺寸与大规模生产。
附图说明
图1为本发明具体实施方式1所获得的莫来石/白榴石多孔陶瓷复合材料的XRD图；
图2为本发明具体实施方式1所获得的莫来石/白榴石多孔陶瓷复合材料的SEM图。
具体实施方式
实施例一：本实施例本发明制备的一种莫来石/白榴石多孔陶瓷复合材料的方法步骤如下：
步骤一、无机聚合物碱激发溶液的制备：将硅溶胶(质量分数30-40％)与氢氧化钾按照摩尔比为1:2混合并磁力混合3天至混合均匀，得到可用于激发活性矿物粉体的无机聚合物碱激发溶液；
步骤二、可发泡的含漂珠/无机聚合物复合浆料配置：将一定质量的偏高岭土粉体加入步骤一所得的无机聚合物碱激发溶液中，加入去离子水调节料浆粘度为100mPa·s，搅拌30分钟，获得硅铝比为2的无机聚合物浆料，再在其中加入漂珠，继续搅拌20分钟，加入双氧水(双氧水/偏高岭土粉体质量比为2％)和十二烷基硫酸钠(十二烷基硫酸钠/偏高岭土粉体质量比为3％)，继续搅拌1-10分钟，获得可发泡的含漂珠/无机聚合物复合浆料。
步骤三、漂珠/泡沫无机聚合物复合材料的固化：将步骤三得到的混合浆料倒入模具中，置于25℃温度下静置24小时发泡。然后将发泡的复合材料置于60℃温度下静置120小时固化，脱模后获得漂珠/泡沫无机聚合物复合材料。
步骤四、莫来石/白榴石多孔陶瓷复合材料陶瓷转化：在一定气氛下，对步骤三获得的漂珠/泡沫无机聚合物复合材料高温处理，升温速度3℃/min，升温至1200℃，保温2小时后降温，降温速度10℃/min冷却至室温，取出后可得莫来石/白榴石多孔陶瓷复合材料。该多孔陶瓷复合材料具有三维网络孔隙结构。
图1为本发明实施例1的步骤四中的莫来石/白榴石多孔陶瓷复合材料的XRD图谱。从图中可以看出，多孔陶瓷复合材料以莫来石和白榴石相为主，莫来石主要是由于漂珠的加入产生的，白榴石来源于基体无机聚合物的高温陶瓷化而得，一定的少量石英相为原料偏高岭土中的杂质，杂志不参与反应并被保留。
图2为本发明实施例1所获得的步骤四中的莫来石/白榴石多孔陶瓷复合材料的SEM图；从SEM图中可以看出，多孔陶瓷复合材料孔隙丰富，具有多种尺度的孔隙结构，孔形以圆形为主，孔分布均匀。
本实施例制得的莫来石/白榴石多孔陶瓷复合材料密度为0.69±0.01g/cm3，抗压强度为4.39±0.52MPa,总孔隙率为69.8±0.2％，开孔孔隙率为67.1±1.3％。
实施例二：本实施例与实施例一不同在于步骤四中升温至1000℃，其它与实施例一相同。
本实施例制得的莫来石/白榴石多孔陶瓷复合材料密度为0.65±0.01g/cm3，抗压强度为4.95±0.32MPa,总孔隙率为68.7±0.5％，开孔孔隙率为60.5±2.0％。
综合以上各数据分析，说明本方法可以成功制备出莫来石/白榴石多孔陶瓷复合材料。

Claims (2)

1.一种莫来石/白榴石多孔陶瓷复合材料的制备方法，其特征在于，包括如下步骤：
步骤一、无机聚合物碱激发溶液的制备：将质量分数30-40%的硅溶胶与氢氧化钾按照摩尔比为1:1.5~3混合并磁力混合3-7天至混合均匀，得到无机聚合物碱激发溶液；
步骤二、可发泡的含漂珠/无机聚合物复合浆料配置：将偏高岭土加入步骤一所得的无机聚合物碱激发溶液中，加入去离子水调节料浆粘度为100mPa·s~500mPa·s之间，搅拌充分，获得硅铝比为2的无机聚合物浆料，再在其中加入漂珠，漂珠与矿物粉体质量比1-5:1，继续搅拌，加入双氧水和十二烷基硫酸钠，其中双氧水与活性矿物粉体质量比为1%-20%，十二烷基硫酸钠与活性矿物粉体质量比为3-10%，继续搅拌，获得可发泡的含漂珠/无机聚合物复合浆料；
步骤三、漂珠/泡沫无机聚合物复合材料的固化：将步骤三得到的混合浆料倒入模具中，置于15-35℃温度下静置6-24小时发泡，再将发泡的复合材料置于40-60℃温度下静置24-120小时固化，脱模后获得漂珠/泡沫无机聚合物复合材料；
步骤四、莫来石/白榴石多孔陶瓷复合材料陶瓷转化：在空气或保护气氛下，对步骤三获得的漂珠/泡沫无机聚合物复合材料高温处理，升温速度1℃/min～5℃/min，升温至900-1300℃，保温2-5小时后降温，降温速度5℃/min～10℃/min冷却至室温，取出后获得莫来石/白榴石多孔陶瓷复合材料。
2.根据权利要求1所述的一种莫来石/白榴石多孔陶瓷复合材料的制备方法，其特征在于，步骤四中升温至1000-1200℃。
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