CN110357604A - 一种轻质泡沫白榴石陶瓷复合材料的制备方法 - Google Patents

一种轻质泡沫白榴石陶瓷复合材料的制备方法 Download PDF

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CN110357604A
CN110357604A CN201910670292.2A CN201910670292A CN110357604A CN 110357604 A CN110357604 A CN 110357604A CN 201910670292 A CN201910670292 A CN 201910670292A CN 110357604 A CN110357604 A CN 110357604A
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inorganic polymer
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闫姝
章凡勇
王帅
冯忠宝
邢鹏飞
杨金龙
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Northeastern University China
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Abstract

本发明公开了一种轻质泡沫白榴石陶瓷复合材料的制备方法,利用无机聚合物前驱体转化法,将白云石微珠作为造孔剂引入可发泡无机聚合物中,富了复合材料多级孔结构,高温处理获得轻质泡沫白榴石陶瓷复合材料。本发明的制备过程为:1.无机聚合物前驱体激发液的制备;2.可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料配置;3.固化成型;4.陶瓷化。本发明克服了多孔白榴石基陶瓷复合材料的绿色制备问题,实现了大尺寸泡沫陶瓷基复合材料的低成本制备,降低了复合材料的密度,提高了强度,获得的材料可用于环境保护,水土保持、吸附过滤等领域。该方法成本低廉,原料来源官方,成型工艺简单,绿色环保无污染,适宜大尺寸大规模生产。

Description

一种轻质泡沫白榴石陶瓷复合材料的制备方法
技术领域
本发明属于泡沫陶瓷复合材料制备领域,涉及一种轻质泡沫白榴石陶瓷复合材料的制备方法,尤其涉及到一种结合空心白云石微珠造孔及无机聚合物高温原位相变转化的轻质泡沫白榴石陶瓷复合材料制备方法。
背景技术
多孔陶瓷的研究始于十九世纪七十年代,它是一种由气孔构成的陶瓷,具有良好的性能,因而备受研究者的关注。常用的制备方法主要有凝胶注模法、有机泡沫浸渍法、直接发泡法、添加造孔剂法等。其中,发泡法具有工艺简单,气孔率高,适合复杂形状等优点,然而孔隙率的提高制约着其强度的提升。造孔剂法是一种相对简单的方式,然而该方法获得的多孔陶瓷虽然强度较高,但是孔隙率较低,且分布不均匀的造孔剂对陶瓷性能也有一定影响。借鉴多孔陶瓷的制备,泡沫无机聚合物可以用作一种陶瓷前驱体用于制备泡沫陶瓷,该方法简单便捷,成本低廉。白云石是一种天然碳酸盐矿物,分子式为CaMg(CO3)2,近似于方解石结构,呈岛状。白云石常被用作于冶金、化工、陶瓷和玻璃等初级产品的原料,通常附加值较低。应用喷雾干燥技术,将白云石粉体制作成空心微珠,可以提高其附加值。此外,近年来其良好的多孔和吸附特性正备受关注。空心微珠作为一种造孔剂在多孔陶瓷制备领域有广泛的应用。无机聚合物材料是一种新型的以硅氧和铝氧四面体结构为主的聚合物材料,在建筑航天和环境等领域都有应用,根据其组成和结构特性,将其在高温处理转化为特性结构的陶瓷材料,成本低廉,工艺简单。
发明内容
本发明针对环境污染治理和材料绿色低成本制备问题,提供了一种轻质泡沫白榴石陶瓷复合材料的制备方法。利用白云石微珠多孔特性,结合无机聚合物高温可陶瓷化的优势,在泡沫无机聚合物中引入白云石空心微珠,并对复合材料高温处理,实现轻质泡沫白榴石陶瓷复合材料的原位制备,复合材料的制备工艺简单、方便便捷、适用范围广,得到的泡沫陶瓷复合材料具有质量轻,强度高的特性,且孔隙可调,可应用于建筑保温、过滤吸附等领域。制备了一种轻质多孔白榴石泡沫陶瓷复合材料及其制备方法,提供了一种轻质多孔白榴石泡沫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:
本发明利用泡沫无机聚合物高温陶瓷转化特性,结合白云石空心微珠可作为造孔剂造孔优势,获得轻质、高强、低密度且孔隙可调节的泡沫白榴石陶瓷复合材料材料,其特点在于:以活性偏高岭土、硅酸盐溶液、白云石微珠为原料、结合无机聚合物转化法和微珠造孔特性,将室温的泡沫无机聚合物复合材料直接高温原位转化为泡沫白榴石陶瓷复合材料。制备过程按照如下步骤进行:
步骤一、无机聚合物前驱体激发液的制备:将质量分数30-40%的硅溶胶与氢氧化钾按照摩尔比为1:1~3,混合并磁力搅拌3-7天,混合均匀后得到无机聚合物前驱体激发液;
步骤二、可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料配置:将活性偏高岭土加入步骤一所得的无机聚合物前驱体激发液中超声辅助搅拌30-45分钟,获得硅/铝比为2的混合料浆,加入去离子水调节料浆粘度为100mPa·s~500mPa·s之间,再加入双氧水和稳泡剂,其中双氧水与偏高岭土质量比为1%-20%,稳泡剂与偏高岭土质量比为0-10%,搅拌5-10分钟,获得可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料;
步骤三、无机聚合物混合浆料的固化成型:将步骤三得到的混合浆料倒入模具中,置于15-30℃温度下静置12-24小时,后置于40-60℃温度下静置24~240小时,脱模后获得白云石微珠/泡沫无机聚合物复合材料;
步骤四、泡沫白榴石的陶瓷化:在空气或保护气氛下,升温速度1℃/min~5℃/min,升温至900-1300℃,到温后保温2-4小时,随炉冷却至室温,即可得到轻质泡沫白榴石陶瓷复合材料。
进一步地,上述步骤四中优选升温至1000-1200℃。
与已有技术相比,本发明的有益效果体现在:
本发明将现有无机聚合物材料视作前驱体,结合了白云石空心微珠造孔剂的结构优势,利用前驱体转化法,对含有白云石微珠的无机聚合物复合体系室温发泡,并高温处理,获得了强度高、质量轻、孔隙率大且孔隙结构可调节的白榴石泡沫陶瓷复合材料。白云石微珠的加入在发泡的基础上更丰富了体系内孔隙的尺度及层次结构。本发明涉及无机聚合物室温发泡合成及高温转化,也对白云石微珠造孔剂的应用起到了一定的扩展。获得的白榴石泡沫陶瓷复合材料具有成本低、工艺简单、形状多样、适用范围广等优点。
附图说明
图1为本发明实施例1所获得的轻质泡沫白榴石陶瓷复合材料的XRD图;
图2为本发明实施例1所获得的轻质泡沫白榴石陶瓷复合材料的SEM图。
具体实施方式
实施例一:本实施例一种轻质泡沫白榴石陶瓷复合材料制备方法的步骤如下:
步骤一、无机聚合物前驱体激发液的制备:将硅溶胶(质量分数40%)与氢氧化钾按照摩尔比为1:2,混合并磁力搅拌3-7天,混合均匀后得到无机聚合物前驱体激发液;
步骤二、可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料配置:将一定质量的活性偏高岭土加入步骤一所得的无机聚合物前驱体激发液中超声辅助搅拌45分钟,获得硅/铝比为2的混合料浆,加入去离子水调节料浆粘度为100mPa·s,再加入双氧水(双氧水/偏高岭土质量比为3%)和稳泡剂(稳泡剂/偏高岭土质量比为3%),搅拌5分钟,获得可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料;
步骤三、无机聚合物混合浆料的固化成型: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,后置于60℃温度下静置7天,脱模后获得白云石微珠/泡沫无机聚合物复合材料。
步骤四、泡沫陶瓷复合材料陶瓷转化:在一定气氛下,升温速度3℃/min,升温至1000℃,到温后保温2小时,随炉冷却至室温,即可得到轻质泡沫白榴石陶瓷复合材料。该泡沫陶瓷复合材料具有多孔结构。
图1为实施例1的步骤四中的轻质泡沫白榴石陶瓷复合材料的XRD图谱。从图中可以看出,陶瓷复合材料以白榴石相为主,有少量方镁石和石灰石相为白云石微珠引入后所致。
图2为实施例1所获得的步骤四中的轻质泡沫白榴石陶瓷复合材料的SEM图;从SEM图中可以看出,复合材料存在不同孔径的孔隙结构。
本实施例制得的轻质泡沫白榴石陶瓷复合材料密度为0.58±0.01g/cm3,抗压强度为4.49±0.37MPa,总孔隙率为76.9±0.4%,开孔孔隙率为70.2±0.1%。
实施例二:本实施例与实施例一不同在于步骤四中升温至1200℃,其它与具体实施方式一相同。
本实施例制得的轻质泡沫白榴石陶瓷复合材料密度为0.58±0.01g/cm3,抗压强度为3.91±0.52MPa,总孔隙率为76.7±0.6%,开孔孔隙率为70.8±1.8%。
综合以上各数据分析,说明本方法成功制备出轻质泡沫白榴石陶瓷复合材料。

Claims (2)

1.一种轻质泡沫白榴石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、无机聚合物前驱体激发液的制备:将质量分数30-40%的硅溶胶与氢氧化钾按照摩尔比为1:1-3,混合并磁力搅拌3-7天,混合均匀后得到无机聚合物前驱体激发液;
步骤二、可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料配置:将活性偏高岭土加入步骤一所得的无机聚合物前驱体激发液中超声辅助搅拌,获得硅/铝比为2的混合料浆,加入去离子水调节料浆粘度为100mPa·s~500mPa·s之间,再加入双氧水和稳泡剂,其中双氧水与偏高岭土质量比为1%-20%,稳泡剂与偏高岭土质量比为0-10%,搅拌,获得可发泡的含白云石空心微珠的无机聚合物前驱体混合浆料;
步骤三、无机聚合物混合浆料的固化成型:将步骤三得到的混合浆料倒入模具中,置于15-30℃温度下静置12-24小时,后置于40-60℃温度下静置24~240小时,脱模后获得白云石微珠/泡沫无机聚合物复合材料;
步骤四、泡沫白榴石的陶瓷化:在空气或保护气氛下,升温速度1℃/min~5℃/min,升温至900-1300℃,到温后保温2-4小时,随炉冷却至室温,即可得到轻质泡沫白榴石陶瓷复合材料。
2.根据权利要求1所述的一种轻质泡沫白榴石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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