CN106747634B - 一种莫来石轻质耐火材料及其制备方法 - Google Patents

一种莫来石轻质耐火材料及其制备方法 Download PDF

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CN106747634B
CN106747634B CN201611104954.2A CN201611104954A CN106747634B CN 106747634 B CN106747634 B CN 106747634B CN 201611104954 A CN201611104954 A CN 201611104954A CN 106747634 B CN106747634 B CN 106747634B
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桑绍柏
舒小妹
李亚伟
徐义彪
王庆虎
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种莫来石轻质耐火材料及其制备方法。其技术方案是：以55～65wt％的高岭土细粉和35～45wt％的活性α‑Al2O3微粉为原料，外加占所述原料0.5～0.7wt％的聚羧酸盐、2.5～3.5wt％的稳泡剂、0.1～0.25wt％的异丁烯/马来酸酐水溶性共聚物、8～10wt％的铝溶胶、40～50wt％的水、0.1～6wt％的造孔剂和1.0～1.40wt％的发泡剂，混合均匀，浇注成型，干燥，在1200～1600℃的条件下保温2～4h，制得莫来石轻质耐火材料。所述高岭土细粉：Al2O3含量＞47wt％，Fe2O3含量＜0.5wt％，CaO含量＜0.07wt％，K2O+Na2O含量＜0.1wt％。本发明具有工艺简单和生坯强度高的特点，所制备的莫来石轻质耐火材料使用温度高、导热系数小和耐压强度较高。

Description

一种莫来石轻质耐火材料及其制备方法
技术领域
本发明属于轻质耐火材料技术领域。尤其涉及一种莫来石轻质耐火材料及其制备方法。
背景技术
莫来石是Al2O3-SiO2系中唯一稳定的二元化合物，它具有熔点高(1850℃)、热膨胀系数低、热导率低和化学稳定性好等特点。以莫来石为主晶相的轻质隔热材料具有抗热震性高和导热系数小等性能，因此莫来石轻质耐火材料被广泛应用在工业窑炉和其他热工设备。
目前，工业制备莫来石轻质保温砖制品的原料主要是煤矸石、焦宝石和蓝晶石尾矿等，所用原料多选用天然原料，其中有害杂质(如：铁、镁和钙等)含量相对较高，所制备的产品纯度不高，导致产品使用温度不高，一般低于1300℃。
轻质隔热材料的制备方法主要有燃尽物加入法、溶胶凝胶法、凝胶注模法和发泡法等。
燃尽物加入法是隔热耐火材料中最常用的生产方法。“莫来石轻质隔热耐火砖及其生产方法”(CN104973869A)的专利技术，以聚苯乙烯球和锯末为燃尽物制备莫来石轻质隔热耐火砖，生产工艺较为复杂，聚苯乙烯小球烧失后产生的气孔不稳定，而且锯末烧失后产生的气孔较大，污染环境。
“一种莫来石轻质隔热砖及其制备方法”(CN103011856B)的专利技术，采用凝胶剂、热固性水溶性高分子化合物和促凝剂，通过凝胶注模的方法制备莫来石轻质隔热砖。这种凝胶注模法所创造的凝胶体系十分复杂，工艺繁琐，并且成本较高。
发泡法制备的成品体积密度小，结构分布均匀且多为封闭的圆形孔，但仍存生坯强度较低，成型过程中容易出现坍塌、成品率低和生产周期长等问题。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种工艺简单和生坯强度高的莫来石轻质耐火材料的制备方法，用该方法制备的莫来石轻质耐火材料使用温度高、导热系数小和耐压强度较高。
为实现上述目的，本发明所采用的技术方案是：以45～65wt％的高岭土细粉和35～55wt％的活性α-Al2O3微粉为原料，外加占所述原料0.1～0.7wt％的减水剂、0.5～3.5wt％的稳泡剂、0～0.25wt％的异丁烯/马来酸酐水溶性共聚物、3～10wt％的铝溶胶、15～50wt％的水、0～9wt％的造孔剂和0.10～1.40wt％的发泡剂，混合均匀，浇注成型，干燥，在1200～1600℃的条件下保温2～4h，制得莫来石轻质耐火材料。
所述高岭土细粉：Al2O3含量＞47wt％，Fe2O3含量＜0.5wt％，CaO含量＜0.07wt％，K2O+Na2O含量＜0.1wt％；所述高岭土细粉的粒径小于0.2mm。
所述活性α-Al2O3微粉中的Al2O3含量≥99wt％，中位径小于1.5μm。
所述减水剂为三聚磷酸钠、六偏磷酸钠和聚羧酸盐中的一种。
所述稳泡剂为淀粉或为糊精。
所述造孔剂为炭黑或为稻壳。
所述异丁烯/马来酸酐水溶性共聚物的分子量为55000～65000。
所述发泡剂为十二烷基硫酸钠、十二烷基苯磺酸钠和十二烷基苯酚聚氧乙烯醚中的一种。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
本发明以高岭土细粉和活性α-Al2O3微粉为原料，混合均匀后浇注成型，干燥，高温烧成后即得到莫来石轻质耐火材料，生产工艺简单。
本发明通过加入异丁烯/马来酸酐水溶性共聚物，在凝胶化过程中不需要加入单体、引发剂和催化剂，在室温条件下即可自发凝胶化，实现泡沫浆料的快速固化成型，与其他凝胶注模工艺相比，其工艺更为简单。同时泡沫浆料的快速固化成型能够使泡沫结构稳定，抑制泡沫成长，从而提高了生坯强度。
本发明所用的高岭土细粉的氧化铝含量较高(Al2O3含量＞47wt％)，杂质较少，如K2O+Na2O含量＜0.1wt％，CaO含量＜0.07wt％，Fe2O3含量＜0.5wt％，所制备的莫来石轻质耐火材料使用温度大幅度提高，其使用温度可达1500℃。
本发明采用复合造孔法，以发泡法为主，材料中的气孔一方面来自于发泡剂造孔，另一方面，在保证生坯不坍塌的情况下，加入一定量的燃尽物，燃尽物烧失后会产生气孔。由于材料的气孔率得到提高，相应的导热系数也会降低。所制备的莫来石轻质耐火材料孔隙尺寸分布均匀，体积密度小。
本发明加入的铝溶胶粒径为纳米级，远远小于固体原料，在高温下促进材料发生固相烧结，形成莫来石网络结构，提高了莫来石轻质耐火材料的耐压强度。
本发明所制备的莫来石轻质耐火材料经检测：体积密度为0.3～1.0g/cm3；显气孔率为65～90％；常温耐压强度为2.0～18.0Mpa；1000℃时的导热系数为0.22～0.43W/(m·k)。
因此，本发明具有工艺简单和生坯强度高的特点，所制备的莫来石轻质耐火材料使用温度高、导热系数小和耐压强度较高。
具体实施方式
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制。
为避免重复，先将本具体实施方式所涉及的原料和外加剂统一描述如下，实施例中不再赘述：
所述高岭土细粉：Al2O3含量＞47wt％，Fe2O3含量＜0.5wt％，CaO含量＜0.07wt％，K2O+Na2O含量＜0.1wt％；所述高岭土细粉的粒径小于0.2mm。
所述活性α-Al2O3微粉中的Al2O3含量≥99wt％，中位径小于1.5μm。
所述异丁烯/马来酸酐水溶性共聚物的分子量为55000～65000。
实施例1
一种莫来石轻质耐火材料及其制备方法。以60～65wt％的高岭土细粉和35～40wt％的活性α-Al2O3微粉为原料，外加占所述原料0.5～0.6wt％的减水剂、2.5～3.0wt％的稳泡剂、0.10～0.20wt％的异丁烯/马来酸酐水溶性共聚物、8～10wt％的铝溶胶、40～45wt％的水、3～6wt％的造孔剂和1.10～1.40wt％的发泡剂，混合均匀，浇注成型，干燥，在1200～1600℃的条件下保温2～4h，制得莫来石轻质耐火材料。
所述减水剂为聚羧酸盐。
所述稳泡剂为糊精。
所述造孔剂为稻壳。
所述发泡剂为十二烷基苯酚聚氧乙烯醚。
本实施例制备的莫来石轻质耐火材料经检测：体积密度为0.4～0.6g/cm3；显气孔率为80～87％；常温耐压强度为4.0～8.0Mpa；1000℃时的导热系数为0.24～0.30W/(m·k)。
实施例2
一种莫来石轻质耐火材料及其制备方法。以55～60wt％的高岭土细粉和40～45wt％的活性α-Al2O3微粉为原料，外加占所述原料0.6～0.7wt％的减水剂、3.0～3.5wt％的稳泡剂、0.15～0.25wt％的异丁烯/马来酸酐水溶性共聚物、9～10wt％的铝溶胶、45～50wt％的水、0.1～3.0wt％的造孔剂和1.0～1.3wt％的发泡剂，混合均匀，浇注成型，干燥，在1200～1600℃的条件下保温2～4h，制得莫来石轻质耐火材料。
所述减水剂为聚羧酸盐。
所述稳泡剂为淀粉。
所述造孔剂为炭黑。
所述发泡剂为十二烷基硫酸钠。
本实施例制备的莫来石轻质耐火材料经检测：体积密度为0.3～0.5g/cm3；显气孔率为83～90％；常温耐压强度为2.0～6.0Mpa；1000℃时的导热系数为0.22～0.28W/(m·k)。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式以高岭土细粉和活性α-Al2O3微粉为原料，混合均匀后浇注成型，干燥，高温烧成后即得到莫来石轻质耐火材料，生产工艺简单。
本具体实施方式通过加入异丁烯/马来酸酐水溶性共聚物，在凝胶化过程中不需要加入单体、引发剂和催化剂，在室温条件下即可自发凝胶化，实现泡沫浆料的快速固化成型，与其他凝胶注模工艺相比，其工艺更为简单。同时泡沫浆料的快速固化成型能够使泡沫结构稳定，抑制泡沫成长，从而提高了生坯强度。
本具体实施方式所用的高岭土细粉的氧化铝含量较高(Al2O3含量＞47wt％)，杂质较少，如K2O+Na2O含量＜0.1wt％，CaO含量＜0.07wt％，Fe2O3含量＜0.5wt％，所制备的莫来石轻质耐火材料使用温度大幅度提高，其使用温度可达1500℃。
本具体实施方式采用复合造孔法，以发泡法为主，材料中的气孔一方面来自于发泡剂造孔，另一方面，在保证生坯不坍塌的情况下，加入一定量的燃尽物，燃尽物烧失后会产生气孔。由于材料的气孔率得到提高，相应的导热系数也会降低。所制备的莫来石轻质耐火材料孔隙尺寸分布均匀，体积密度小。
本具体实施方式加入的铝溶胶粒径为纳米级，远远小于固体原料，在高温下促进材料发生固相烧结，形成莫来石网络结构，提高了莫来石轻质耐火材料的耐压强度。
本具体实施方式所制备的莫来石轻质耐火材料体积密度为0.3～1.0g/cm3，显气孔率为65～90％，常温耐压强度为2.0～18.0Mpa，1000℃时的导热系数为0.22～0.43W/(m·k)。
因此，本具体实施方式具有工艺简单和生坯强度高的特点，所制备的莫来石轻质耐火材料使用温度高、导热系数小和耐压强度较高。

Claims (5)

1.一种莫来石轻质耐火材料的制备方法，其特征在于：以55～65wt％的高岭土细粉和35～45wt％的活性α-Al2O3微粉为原料，外加占所述原料0.5～0.7wt％的聚羧酸盐、2.5～3.5wt％的稳泡剂、0.1～0.25wt％的异丁烯/马来酸酐水溶性共聚物、8～10wt％的铝溶胶、40～50wt％的水、0.1～6wt％的造孔剂和1.0～1.40wt％的发泡剂，混合均匀，浇注成型，干燥，在1200～1600℃的条件下保温2～4h，制得莫来石轻质耐火材料；
所述高岭土细粉：Al2O3含量＞47wt％，Fe2O3含量＜0.5wt％，CaO含量＜0.07wt％，K2O+Na2O含量＜0.1wt％；所述高岭土细粉的粒径小于0.2mm；
所述活性α-Al2O3微粉中的Al2O3含量≥99wt％，中位径小于1.5μm；
所述异丁烯/马来酸酐水溶性共聚物的分子量为55000～65000。
2.根据权利要求1所述的莫来石轻质耐火材料的制备方法，其特征在于所述稳泡剂为淀粉或为糊精。
3.根据权利要求1所述的莫来石轻质耐火材料的制备方法，其特征在于所述造孔剂为炭黑或为稻壳。
4.根据权利要求1所述的莫来石轻质耐火材料的制备方法，其特征在于所述发泡剂为十二烷基硫酸钠、十二烷基苯磺酸钠和十二烷基苯酚聚氧乙烯醚中的一种。
5.一种莫来石轻质耐火材料，其特征在于所述莫来石轻质耐火材料是根据权利要求1～4项中任一项所述的莫来石轻质耐火材料的制备方法所制备的莫来石轻质耐火材料。
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