CN110204309A - 一种含锆堇青石莫来石复相材料及其制备方法 - Google Patents

一种含锆堇青石莫来石复相材料及其制备方法 Download PDF

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CN110204309A
CN110204309A CN201910475596.3A CN201910475596A CN110204309A CN 110204309 A CN110204309 A CN 110204309A CN 201910475596 A CN201910475596 A CN 201910475596A CN 110204309 A CN110204309 A CN 110204309A
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cordierite
containing zirconium
mullite
composite diphase
preparation
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李远兵
李仕祺
向若飞
李淑静
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Abstract

本发明涉及一种含锆堇青石莫来石复相材料及其制备方法。其技术方案是：先以3.0～32.0wt％的粘土、19.0～30.0wt％的滑石粉和40.0～75.0wt％的蓝晶石尾矿为原料，外加所述原料150～200wt％的水、3～6wt％的聚乙烯醇、0.5～2.0wt％的氧化钛和0.5～2.0wt％的氧化钇，球磨4～10h，得到混合料；再将所述混合料机压成型，干燥，在1300～1420℃条件下保温3～7h，自然冷却，制得含锆堇青石莫来石复相材料。所述蓝晶石尾矿的化学成分是：SiO2含量≥35.6wt％，Al2O3含量≥50.0wt％，ZrSiO4≥10.4wt％。本发明具有资源化程度高、环境友好、工艺简单和生产成本低的特点；所制备的含锆堇青石莫来石复相材料线变化率小、耐压强度大和使用温度高。

Description

一种含锆堇青石莫来石复相材料及其制备方法
技术领域
本发明属于堇青石莫来石复相材料技术领域。具体涉及一种含锆堇青石莫来石复相材料及其制备方法。
背景技术
蓝晶石尾矿是锆英石选矿后得到的产物，主要成分为蓝晶石并残留锆英石的高附加值原料。作为选矿后的工业残留物，蓝晶石尾矿中的锆英石极具利用价值，但是尾矿若处理不当不仅占用土地资源，且会带来严重的环境污染。
堇青石具有热膨胀系数小好等优点，但由于韧性较低、荷重软化点低和合成范围窄，从而限制了它优良性能的发挥。而莫来石虽高温性能优良和机械强度大，但热膨胀系数较大。因此为兼顾材料的高温性能，将堇青石与莫来石进行复合是提高材料性能最有效的措施之一。
目前，已有制备堇青石莫来石复相材料的技术，如“堇青石-莫来石复相材料的原位反应烧成的制备方法”(CN101519304A)专利技术，公开了一种以高岭土、滑石和工业氧化铝为主要原料制备堇青石莫来石复相材料的技术，其中高岭土所占比例最大。高岭土烧失很大，原料中的高岭土在烧成过程中会产生大量的孔洞，并且添加了五氧化二钒作为烧结助剂，增加了制造成本；“一种用蓝晶石合成堇青石-莫来石复相材料的方法”(CN103896605A)专利技术，该技术以蓝晶石和滑石为原料制备堇青石-莫来石复相材料，所制备的样品体积密度较大，气孔率较小，因此隔热效果较差，不利于节能环保；“一种碳化硅增强堇青石-莫来石陶瓷复合材料及其制备方法”(CN107619267A)专利技术，该技术以堇青石、莫来石、膨润土、碳化硅和碳化硼为原料制备碳化硅增强堇青石-莫来石复相材料，所制备的样品体积密度较大，且常温耐压强度较低，工艺较为复杂。“一种用煤矸石合成堇青石-莫来石复合材料的方法”(CN101508563A)专利技术，该技术以煤矸石、镁碳砖、滑板砖反应合成堇青石-莫来石复相材料，煤矸石中含有10～20wt％的C，在高温处理过程中形成大量孔洞，导致烧成过程中坯体内部温度分布不均匀，由于堇青石的烧成温度区间窄，温度分布不均会引起坯体开裂，影响制品的成品率。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种资源化程度高、环境友好、工艺简单和生产成本低的含锆堇青石莫来石复相材料的制备方法。用该方法所制备的含锆堇青石莫来石复相材料的线变化率小、耐压强度大、使用温度高和产业化前景大。
为实现上述目的，本发明采用的技术方案是：先以3.0～32.0wt％的粘土、19.0～30.0wt％的滑石粉和40.0～75.0wt％的蓝晶石尾矿为原料，外加所述原料150～200wt％的水、3～6wt％的聚乙烯醇、0.5～2.0wt％的氧化钛和0.5～2.0wt％的氧化钇，球磨4～10h，得到混合料；将所述混合料机压成型，干燥，在1300～1420℃条件下保温3～7h，自然冷却，制得含锆堇青石莫来石复相材料。
所述粘土的粒径小于0.074mm；粘土的化学成分是：SiO2含量≥45.0wt％，Al2O3含量≥32.0wt％，烧失量≤16.0wt％。
所述滑石粉的粒径小于0.088mm；滑石粉的化学成分是：MgO含量≥38.0wt％，SiO2含量≥40.0wt％，烧失量≤20.0wt％。
所述蓝晶石尾矿的粒径小于0.1mm；蓝晶石尾矿的化学成分是：SiO2含量≥35.6wt％，Al2O3含量≥50.0wt％，ZrSiO4≥10.4wt％。
所述机压的压强为50～100MPa。
由于采用上述技术方案，本发明与现有技术相比具有以下积极效果：
1、本发明以蓝晶石尾矿为主要原料，解决了蓝晶石尾矿的存放问题，节约了成本，并且将蓝晶石尾矿资源再生利用，故生产成本低、环境友好和产业化前景大。
2、本发明采用的蓝晶石尾矿含有的锆英石能扩大堇青石莫来石复相材料的烧成范围，由于堇青石的烧成温度区间窄，温度分布不均会引起坯体开裂，因此提高了含锆堇青石莫来石复相材料的成品率。
3、本发明制备的含锆堇青石莫来石复相材料具有低的体积密度、高的气孔率和高的强度，本发明因此保温效果好、性能优良和节能环保。
本发明所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.50～1.82g/cm3，显气孔率为26.6％～32.8％，耐压强度为123～198MPa，线变化率为0.45～1.08％，使用温度高达1400℃。
因此，本发明具有资源化程度高、环境友好、工艺简单和生产成本低的特点；所制备的含锆堇青石莫来石复相材料的线变化率小、耐压强度大、使用温度高和产业化前景大。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述，并非对本发明保护范围的限制。
为避免重复，先将本具体实施方式所涉及到的技术参数统一描述如下，实施例中不再赘述：
所述粘土的粒径小于0.074mm；粘土的化学成分是：SiO2含量≥45.0wt％，Al2O3含量≥32.0wt％，烧失量≤16.0wt％。
所述滑石粉的粒径小于0.088mm；滑石粉的化学成分是：MgO含量≥38.0wt％，SiO2含量≥40.0wt％，烧失量≤20.0wt％。
所述蓝晶石尾矿的粒径小于0.1mm；蓝晶石尾矿的化学成分是：SiO2含量≥35.6wt％，Al2O3含量≥50.0wt％，ZrSiO4≥10.4wt％。
实施例1
一种含锆堇青石莫来石复相材料及其制备方法。先以3.0～8.0wt％的粘土、21.0～24.0wt％的滑石粉和68.0～75.0wt％的蓝晶石尾矿为原料，外加所述原料150～160wt％的水、3～4wt％的聚乙烯醇、0.5～1.0wt％的氧化钛和0.5～1.0wt％的氧化钇，球磨4～6h，得到混合料；再将所述混合料机压成型，干燥，在1300～1324℃条件下保温3～5h，自然冷却，制得含锆堇青石莫来石复相材料。
本实施例中，机压成型的压强为50～60MPa。
本实施例所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.50～1.74g/cm3，显气孔率为27.5～32.8％，耐压强度为123～154MPa，线变化率为0.67～1.05％。
实施例2
一种含锆堇青石莫来石复相材料及其制备方法。先以8.0～14.0wt％的粘土、23.0～26.0wt％的滑石粉和61.0～68.0wt％的蓝晶石尾矿为原料，外加所述原料160～170wt％的水、4～5wt％的聚乙烯醇、1.0～1.5wt％的氧化钛和1.0～1.5wt％的氧化钇，球磨6～8h，得到混合料；再将所述混合料机压成型，干燥，在1324～1348℃条件下保温5～7h，自然冷却，制得含锆堇青石莫来石复相材料。
本实施例中，机压成型的压强为60～70MPa。
本实施例所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.63～1.79g/cm3，显气孔率为26.9～30.4％，耐压强度为137～165MPa，线变化率为0.63～0.92％。
实施例3
一种含锆堇青石莫来石复相材料及其制备方法。先以14.0～20.0wt％的粘土、24.0～28.0wt％的滑石粉和54.0～61.0wt％的蓝晶石尾矿为原料，外加所述原料170～180wt％的水、5～6wt％的聚乙烯醇、1.5～2.0wt％的氧化钛和1.5～2.0wt％的氧化钇，球磨8～10h，得到混合料；再将所述混合料机压成型，干燥，在1348～1372℃条件下保温3～5h，自然冷却，制得含锆堇青石莫来石复相材料。
本实施例中，机压成型的压强为70～80MPa。
本实施例所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.67～1.82g/cm3，显气孔率为26.6～29.5％，耐压强度为146～198MPa，线变化率为0.45～0.82％。
实施例4
一种含锆堇青石莫来石复相材料及其制备方法。先以20.0～30.0wt％的粘土、27.0～30.0wt％的滑石粉和40.0～50.0wt％的蓝晶石尾矿为原料，外加所述原料180～190wt％的水、3～4wt％的聚乙烯醇、0.5～1.0wt％的氧化钛和0.5～1.0wt％的氧化钇，球磨4～6h，得到混合料；再将所述混合料机压成型，干燥，在1372～1396℃条件下保温5～7h，自然冷却，制得含锆堇青石莫来石复相材料。
本实施例中，机压成型的压强为80～90MPa。
本实施例所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.55～1.78g/cm3，显气孔率为27.1～31.7％，耐压强度为139～182MPa，线变化率为0.59～0.94％。
实施例5
一种含锆堇青石莫来石复相材料及其制备方法。先以26.0～32.0wt％的粘土、19.0～22.0wt％的滑石粉和47.0～54.0wt％的蓝晶石尾矿为原料，外加所述原料190～200wt％的水、4～5wt％的聚乙烯醇、1.0～1.5wt％的氧化钛和1.0～1.5wt％的氧化钇，球磨6～8h，得到混合料；再将所述混合料机压成型，干燥，在1396～1420℃条件下保温3～5h，自然冷却，制得含锆堇青石莫来石复相材料。
本实施例中，机压成型的压强为90～100MPa。
本实施例所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.52～1.68g/cm3，显气孔率为28.5～32.4％，耐压强度为134～176MPa，线变化率为0.71～1.08％。
本具体实施方式与现有技术相比具有以下积极效果：
1、本具体实施方式以蓝晶石尾矿为主要原料，解决了蓝晶石尾矿的存放问题，节约了成本，并且将蓝晶石尾矿资源再生利用，故生产成本低、环境友好和产业化前景大。
2、本具体实施方式采用的蓝晶石尾矿含有的锆英石能扩大堇青石莫来石复相材料的烧成范围，由于堇青石的烧成温度区间窄，温度分布不均会引起坯体开裂，因此提高了含锆堇青石莫来石复相材料的成品率。
3、本具体实施方式制备的含锆堇青石莫来石复相材料具有低的体积密度、高的气孔率和高的强度，本具体实施方式因此保温效果好、性能优良和节能环保。
本具体实施方式所制备的含锆堇青石莫来石复相材料经X射线衍射分析，主晶相为堇青石，次晶相为莫来石和锆英石。经检测：体积密度为1.50～1.82g/cm3，显气孔率为26.6％～32.8％，耐压强度为123～198MPa，线变化率为0.45～1.08％，使用温度高达1400℃。
因此，本具体实施方式具有资源化程度高、环境友好、工艺简单和生产成本低的特点；所制备的含锆堇青石莫来石复相材料的线变化率小、耐压强度大、使用温度高和产业化前景大。

Claims (6)

1.一种含锆堇青石莫来石复相材料的制备方法，其特征在于：先以3.0～32.0wt％的粘土、19.0～30.0wt％的滑石粉和40.0～75.0wt％的蓝晶石尾矿为原料，外加所述原料150～200wt％的水、3～6wt％的聚乙烯醇、0.5～2.0wt％的氧化钛和0.5～2.0wt％的氧化钇，球磨4～10h，得到混合料；再将所述混合料机压成型，干燥，在1300～1420℃条件下保温3～7h，自然冷却，制得含锆堇青石莫来石复相材料。
2.根据权利要求1所述的含锆堇青石莫来石复相材料的制备方法，其特征在于所述粘土的粒径小于0.074mm；粘土的化学成分是：SiO2含量≥45.0wt％，Al2O3含量≥32.0wt％，烧失量≤16.0wt％。
3.根据权利要求1所述的含锆堇青石莫来石复相材料的制备方法，其特征在于所述滑石粉的粒径小于0.088mm；滑石粉的化学成分是：MgO含量≥38.0wt％，SiO2含量≥40.0wt％，烧失量≤20.0wt％。
4.根据权利要求1所述的含锆堇青石莫来石复相材料的制备方法，其特征在于所述蓝晶石尾矿的粒径小于0.1mm；蓝晶石尾矿的化学成分是：SiO2含量≥35.6wt％，Al2O3含量≥50.0wt％，ZrSiO4≥10.4wt％。
5.根据权利要求1所述的含锆堇青石莫来石复相材料的制备方法，其特征在于所述机压的压强为50～100MPa。
6.一种含锆堇青石莫来石复相材料，其特征在于所述含锆堇青石莫来石复相材料是根据权利要求1～5项中任一项所述含锆堇青石莫来石复相材料的制备方法所制备的含锆堇青石莫来石复相材料。
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