CN108033794A - 一种轻质隔热耐火陶瓷材料的制备方法 - Google Patents

一种轻质隔热耐火陶瓷材料的制备方法 Download PDF

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CN108033794A
CN108033794A CN201711172472.5A CN201711172472A CN108033794A CN 108033794 A CN108033794 A CN 108033794A CN 201711172472 A CN201711172472 A CN 201711172472A CN 108033794 A CN108033794 A CN 108033794A
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鲁庭志
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MA'ANSHAN LIRUN METALLURGY MATERIAL CO Ltd
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Abstract

本发明公开了一种轻质隔热耐火陶瓷材料的制备方法，首先在莫来石纤维表面涂覆ZrO2涂层，以煤矸石为主原料制备堇青石粉体，之后通过凝胶注模成型技术，制备了具有ZrO2/莫来石纤维包覆结构的堇青石‑莫来石耐火陶瓷材料。本发明中通过溶胶‑凝胶法在莫来石纤维表面包覆ZrO2涂层，保证在球磨工艺下莫来石纤维结构完整性良好，多孔性能不被破坏，避免了高温下莫来石纤维与基体发生界面反应，纤维在隔热耐火材料内部无序排列，具有较高的孔隙率，同时采用凝胶注模成型技术可以通过控制预混浆中的固含量，调控最终陶瓷的气孔分布状态，提高产品的轻质隔热性能及机械性能，具有优良的抗热震稳定性、高温力学性能和化学稳定性。

Description

一种轻质隔热耐火陶瓷材料的制备方法
技术领域
本发明涉及耐火材料技术领域，具体涉及一种轻质隔热耐火陶瓷材料的制备方法。
背景技术
到目前为止，研制生产的陶瓷纤维耐火材料，其工艺过程基本上是将陶瓷纤维棉破碎后直接掺入各种不定型耐火散料中，经浇注成型。破碎的陶瓷纤维分散度不好，大多都以云片状或团絮状大小不均匀的形式存在。虽然陶瓷纤维浇注料轻型隔热，但是陶瓷纤维在与耐火散状料混合后纤维的多孔性能大多被破坏，多处被耐火泥浆灌满，直接影响到产品的整体强度和最佳隔热效果。
莫来石纤维使用温度在1500-1600℃，特别是高温抗蠕变性和抗热震性能优异，耐热、耐腐蚀和绝热性能极佳。可以用作耐热构件、高温绝热材料。莫来石纤维与陶瓷基体界面热膨胀率和导热率非常接近，莫来石纤维的加入可以提高陶瓷基体的韧性、增加冲击强度，往往为耐热复合材料研发的首选。为避免高温下莫来石纤维与基体发生界面反应，对纤维表面进行改性即表面涂层是目前比较实用有效的方法。
发明内容
本发明提供了一种轻质隔热耐火陶瓷材料的制备方法。
本发明是通过以下技术方案实现的：
一种轻质隔热耐火陶瓷材料的制备方法，首先在莫来石纤维表面涂覆ZrO2涂层，以煤矸石为主原料制备堇青石粉体，之后通过凝胶注模成型技术，制备了具有ZrO2/莫来石纤维包覆结构的堇青石-莫来石耐火陶瓷材料。
其中，所述ZrO2涂层是以Zr(OH)4水凝胶的方式引入，通过溶胶-凝胶工艺将其涂覆在莫来石纤维表面。
具体工艺步骤如下：
（1）凝胶包覆莫来石纤维：
取16-25份ZrOCl2·8H2O为原料，加入至适量蒸馏水中，加入3-6份聚乙二醇作为分散剂，加入3% Y(NO3)3为稳定剂，搅拌均匀后，加入8-15份莫来石纤维，搅拌分散15-30分钟，超声分散8-15分钟，滴加浓氨水直至溶液的pH值至9-10，陈化10-15小时后，用蒸馏水反复洗涤3-5次，然后采用无水乙醇进行醇水交换，制得凝胶浓度折合ZrO2含量在8-10wt%的凝胶包覆莫来石纤维；
（2）堇青石粉体的制备：
将32-54份煤矸石破碎、球磨后过80目筛，然后进行脱碳处理，将脱碳后的煤矸石与氧化物原料置于行星式球磨机中球磨混合后，在箱式电阻炉中于1150-1250℃保温3-5小时，合成堇青石粉体；
（3）预混浆料的制备：
将有机单体丙烯酰胺与交联剂N,N-亚甲基双丙烯酰胺按照20:1的摩尔比加入到去离子水中得到预混液，再加入粉体质量0.3%的分散剂柠檬酸铵，并用氨水将调节pH至8.5-9.5，再加入浆料质量1-2%的聚乙烯醇，得到预混浆料；
（4）注模成型：
将步骤（2）堇青石粉体与步骤（1）凝胶包覆莫来石纤维加入到上述预混浆料中，球磨15-25小时后，加入预混浆料0.5-1%的催化剂TMEDA和0.8-1.5%过硫酸铵，搅拌均匀后注模，室温下固化2-5小时，进行凝胶化；
（5）干燥烧结：
将脱模后材料阴干2-3天，然后在30-45℃中鼓风干燥18-25小时，再于1350-1420℃温度下烧结3-6小时，即得到堇青石-莫来石复相材料，冷却后取出，即可。
其中，所述步骤（2）中氧化物原料是由氧化铝、氧化镁与氧化硅按照2-3:1:4-6的质量比组成。
其中，所述步骤（2）中所述氧化物原料与煤矸石的质量比为1:1。
其中，所述莫来石纤维直径在3-5μm，长度在20-80mm。
本发明有益效果如下：
本发明中通过溶胶-凝胶法在莫来石纤维表面包覆Zr(OH)4凝胶，保证在注模成型前的球磨工艺下莫来石纤维结构完整性较好，纤维不易发生团絮现象，在浆料内分散均匀，再经干燥烧结后，在莫来石纤维表面形成ZrO2保护层，纤维得到较好保护，多孔性能不被破坏，为避免高温下莫来石纤维与基体发生界面反应，提高材料的化学稳定性，改善了堇青石-莫来石复合材料的力学性能；纤维在隔热耐火材料内部无序排列，形成了三维网络结构，具有较高的孔隙率，同时采用凝胶注模成型技术可以通过控制预混浆中的固含量，调控最终陶瓷的气孔分布状态，提高产品的轻质隔热性能；此外Zr(OH)4凝胶具有良好的分散性，在预料中可以起到结合剂的作用，促进凝胶化成型，有助于材料的烧结，产品具有优良的抗热震稳定性、高温力学性能和化学稳定性。
具体实施方式
一种轻质隔热耐火陶瓷材料的制备方法，首先在莫来石纤维表面涂覆ZrO2涂层，以煤矸石为主原料制备堇青石粉体，之后通过凝胶注模成型技术，制备了具有ZrO2/莫来石纤维包覆结构的堇青石-莫来石耐火陶瓷材料。
其中，所述ZrO2涂层是以Zr(OH)4水凝胶的方式引入，通过溶胶-凝胶工艺将其涂覆在莫来石纤维表面。
具体工艺步骤如下：
（1）凝胶包覆莫来石纤维：
取20份ZrOCl2·8H2O为原料，加入至适量蒸馏水中，加入4份聚乙二醇作为分散剂，加入3% Y(NO3)3为稳定剂，搅拌均匀后，加入11份莫来石纤维，搅拌分散30分钟，超声分散15分钟，滴加浓氨水直至溶液的pH值至9-10，陈化12小时后，用蒸馏水反复洗涤5次，然后采用无水乙醇进行醇水交换，制得凝胶浓度折合ZrO2含量在10wt%的凝胶包覆莫来石纤维；
（2）堇青石粉体的制备：
将48份煤矸石破碎、球磨后过80目筛，然后进行脱碳处理，将脱碳后的煤矸石与氧化物原料置于行星式球磨机中球磨混合后，在箱式电阻炉中于1200℃保温4小时，合成堇青石粉体；
（3）预混浆料的制备：
将有机单体丙烯酰胺与交联剂N,N-亚甲基双丙烯酰胺按照20:1的摩尔比加入到去离子水中得到预混液，再加入粉体质量0.3%的分散剂柠檬酸铵，并用氨水将调节pH至9.2，再加入浆料质量1.5%的聚乙烯醇，得到预混浆料；
（4）注模成型：
将步骤（2）堇青石粉体与步骤（1）凝胶包覆莫来石纤维加入到上述预混浆料中，机械搅拌22小时后，加入预混浆料0.8%的催化剂TMEDA和0.9%过硫酸铵，搅拌均匀后注模，室温下固化4小时，进行凝胶化；
（5）干燥烧结：
将脱模后材料阴干2天，然后在40℃中鼓风干燥24小时，再于1380℃温度下烧结4小时，即得到堇青石-莫来石复相材料，冷却后取出，即可。
其中，所述步骤（2）中氧化物原料是由氧化铝、氧化镁与氧化硅按照3:1:5的质量比组成。
其中，所述步骤（2）中所述氧化物原料与煤矸石的质量比为1:1。
其中，所述莫来石纤维直径在3-5μm，长度在20-80mm。

Claims (6)

1.一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，首先在莫来石纤维表面涂覆ZrO2涂层，以煤矸石为主原料制备堇青石粉体，之后通过凝胶注模成型技术，制备了具有ZrO2/莫来石纤维包覆结构的堇青石-莫来石耐火陶瓷材料。
2.根据权利要求1所述的一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，所述ZrO2涂层是以Zr(OH)4水凝胶的方式引入，通过溶胶-凝胶工艺将其涂覆在莫来石纤维表面。
3.根据权利要求1所述的一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，具体工艺步骤如下：
（1）凝胶包覆莫来石纤维：
取16-25份ZrOCl2·8H2O为原料，加入至适量蒸馏水中，加入3-6份聚乙二醇作为分散剂，加入3% Y(NO3)3为稳定剂，搅拌均匀后，加入8-15份莫来石纤维，搅拌分散15-30分钟，超声分散8-15分钟，滴加浓氨水直至溶液的pH值至9-10，陈化10-15小时后，用蒸馏水反复洗涤3-5次，然后采用无水乙醇进行醇水交换，制得凝胶浓度折合ZrO2含量在8-10wt%的凝胶包覆莫来石纤维；
（2）堇青石粉体的制备：
将32-54份煤矸石破碎、球磨后过80目筛，然后进行脱碳处理，将脱碳后的煤矸石与氧化物原料置于行星式球磨机中球磨混合后，在箱式电阻炉中于1150-1250℃保温3-5小时，合成堇青石粉体；
（3）预混浆料的制备：
将有机单体丙烯酰胺与交联剂N,N-亚甲基双丙烯酰胺按照20:1的摩尔比加入到去离子水中得到预混液，再加入粉体质量0.3%的分散剂柠檬酸铵，并用氨水将调节pH至8.5-9.5，再加入浆料质量1-2%的聚乙烯醇，得到预混浆料；
（4）注模成型：
将步骤（2）堇青石粉体与步骤（1）凝胶包覆莫来石纤维加入到上述预混浆料中，球磨15-25小时后，加入预混浆料0.5-1%的催化剂TMEDA和0.8-1.5%过硫酸铵，搅拌均匀后注模，室温下固化2-5小时，进行凝胶化；
（5）干燥烧结：
将脱模后材料阴干2-3天，然后在30-45℃中鼓风干燥18-25小时，再于1350-1420℃温度下烧结3-6小时，即得到堇青石-莫来石复相材料，冷却后取出，即可。
4.根据权利要求3所述的一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，所述步骤（2）中氧化物原料是由氧化铝、氧化镁与氧化硅按照2-3:1:4-6的质量比组成。
5.根据权利要求3所述的一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，所述步骤（2）中所述氧化物原料与煤矸石的质量比为1:1。
6.根据权利要求1、3所述的一种轻质隔热耐火陶瓷材料的制备方法，其特征在于，所述莫来石纤维直径在3-5μm，长度在20-80mm。
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CN109020593A (zh) * 2018-09-08 2018-12-18 佛山皖和新能源科技有限公司 一种弹性耐高温陶瓷隔热瓦及其制备方法
CN111942570A (zh) * 2020-08-14 2020-11-17 中国航空工业集团公司沈阳飞机设计研究所 隔热承载一体化结构及其隔热纤维材料填充结构、方法
CN117886616A (zh) * 2023-12-20 2024-04-16 安徽瑞泰新材料科技有限公司 一种锂电回收回转窑耐火用无水泥浇注料及其制备方法
CN118812268A (zh) * 2024-07-24 2024-10-22 哈尔滨工业大学 一种C/ZrO2复合涂层改性纤维莫来石先驱体的制备方法
CN118812268B (zh) * 2024-07-24 2025-10-28 哈尔滨工业大学 一种C/ZrO2复合涂层改性纤维莫来石先驱体的制备方法
CN121377798A (zh) * 2025-12-24 2026-01-23 弘祥中科(辽宁)耐材有限公司 一种石英石基钢包耐火浇筑材料及其制备工艺

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