CN112028642B - 氧化锆耐火材料及其制备方法 - Google Patents

氧化锆耐火材料及其制备方法 Download PDF

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CN112028642B
CN112028642B CN202010771672.8A CN202010771672A CN112028642B CN 112028642 B CN112028642 B CN 112028642B CN 202010771672 A CN202010771672 A CN 202010771672A CN 112028642 B CN112028642 B CN 112028642B
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李金仁
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Shandong Jinshanhe New Material Technology Co ltd
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Abstract

本发明属于耐火材料技术领域，具体的涉及一种氧化锆耐火材料及其制备方法。以重量份数计，原料组成如下：电熔单斜氧化锆65‑70份、富铝尖晶石10‑12份、焦宝石15‑18份、刚玉粉5‑8份、碱式碳酸镁2.5‑3.0份、单质硅8‑12份、氧化钛0.8‑1.2份、氧化硼2‑3份、氧化钇0.8‑1.2份、添加剂0.8‑1.0份、分散剂2.5‑3.5份和结合剂5‑12份。本发明所述的氧化锆耐火材料，具有耐压强度高、热稳定性高、热震稳定性高、使用寿命长、使用过程中不开裂等特点；所述的氧化锆耐火材料的制备方法，原料易得，生产工艺简单，易操作，生产效率高。

Description

氧化锆耐火材料及其制备方法
技术领域
本发明属于耐火材料技术领域，具体的涉及一种氧化锆耐火材料及其制备方法。
背景技术
氧化锆是一种耐高温、耐腐蚀、耐磨损而且化学性质不活泼的无机非金属材料，尤其是其优良的耐高温、耐腐蚀性能倍受科研工作者的青睐，在20世纪20年代初即被应用于耐火材料领域。
但是，由于二氧化锆单斜型与四方型之间的可逆转变伴有体积效应，造成耐火材料烧成时容易开裂，因此单用纯氧化锆就很难制造出烧结而又不开裂的制品。现有的氧化锆高温耐火材料一般是通过向氧化锆中加入一定量的稳定元素氧化物的方式来实现。
采用上述方式制备得到的氧化锆制品，在使用过程中容易出现开裂、热稳定性差、脱溶等现象，材料的性能难以稳定和保证，使得制备的氧化锆耐火材料无法应用于多种场合，严重限制了氧化锆耐火材料的使用。
发明内容
本发明的目的是：提供一种氧化锆耐火材料，该氧化锆耐火材料性能稳定，使用过程中不开裂，热稳定性好；本发明同时提供了其制备方法。
本发明所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆65-70份、富铝尖晶石10-12份、焦宝石15-18份、刚玉粉5-8份、碱式碳酸镁2.5-3.0份、单质硅8-12份、氧化钛0.8-1.2份、氧化硼2-3份、氧化钇0.8-1.2份、添加剂0.8-1.0份、分散剂2.5-3.5份和结合剂5-12份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2≥99％，余量为杂质。
富铝尖晶石中Al2O3的质量含量＞85wt％。
焦宝石的化学组成为：Al2O3 45-46％、SiO2 51-53％、Fe2O3 0.8-1.2％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
优选的，以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈30-35％、聚乙二醇30-35％和羧甲基丙烯酰胺35-40％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
优选的，以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇35-45％、亚甲基双丙烯酰胺25-35％和钼酚醛树脂25-35％。
添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物。
聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.5-1.3:1。
本发明所述的氧化锆耐火材料的制备方法，由以下步骤组成：
(1)将电熔单斜氧化锆、富铝尖晶石和焦宝石粉碎至0.025-0.03mm；
(2)将电熔单斜氧化锆、富铝尖晶石、焦宝石、刚玉粉、碱式碳酸镁、单质硅、氧化钛、氧化硼、氧化钇与分散剂混合均匀，得到预混料；
(3)将预混料与结合剂搅拌混合，并放入模具中压制形成坯体，坯体于750-850℃下烘干；
(4)将烘干后的坯体浸渍添加剂溶液，于180-200℃进行固化，然后于烧结炉中进行高温烧结，冷却至室温，制备得到氧化锆耐火材料。
其中：
步骤(3)中所述的压制成型为首先进行干压成型，然后进行冷等静压成型，干压成型压力为50-55Mpa，保压时间为25-35s，然后进行冷等静压成型，压强为30-35MPa，保压时间为60-80s。
步骤(4)中所述于1750-1850℃煅烧2.5-3h进行高温烧结。
本发明与现有技术相比，具有以下有益效果：
(1)本发明所述的氧化锆耐火材料，具有耐压强度高、热稳定性高、热震稳定性高、使用寿命长、使用过程中不开裂等特点。
(2)本发明所述的氧化锆耐火材料的制备方法，原料易得，生产工艺简单，易操作，生产效率高。
具体实施方式
以下结合实施例对本发明作进一步描述。
实施例1
本实施例1所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆68份、富铝尖晶石12份、焦宝石17份、刚玉粉6份、碱式碳酸镁2.5份、单质硅8份、氧化钛0.8份、氧化硼2份、氧化钇0.8份、添加剂0.8份、分散剂3.0份和结合剂8份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2为99％，余量为杂质。
富铝尖晶石中Al2O3的质量含量为88wt％。
焦宝石的化学组成为：Al2O346％、SiO2 52％、Fe2O31.0％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈30％、聚乙二醇35％和羧甲基丙烯酰胺35％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇35％、亚甲基双丙烯酰胺30％和钼酚醛树脂35％。
添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物。
聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.3:1。
本实施例1所述的氧化锆耐火材料的制备方法，由以下步骤组成：
(1)将电熔单斜氧化锆、富铝尖晶石和焦宝石粉碎至0.03mm；
(2)将电熔单斜氧化锆、富铝尖晶石、焦宝石、刚玉粉、碱式碳酸镁、单质硅、氧化钛、氧化硼、氧化钇与分散剂混合均匀，得到预混料；
(3)将预混料与结合剂搅拌混合，并放入模具中压制形成坯体，坯体于750℃下烘干；
(4)将烘干后的坯体浸渍添加剂溶液，于180℃进行固化，然后于烧结炉中进行高温烧结，冷却至室温，制备得到氧化锆耐火材料。
其中：
步骤(3)中所述的压制成型为首先进行干压成型，然后进行冷等静压成型，干压成型压力为55Mpa，保压时间为25s，然后进行冷等静压成型，压强为35MPa，保压时间为70s。
步骤(4)中所述于1850℃煅烧2.5h进行高温烧结。
对实施例1制备的氧化锆耐火材料进行性能测试，1800℃下热膨胀率为0.56％，常温耐压为423MPa。
实施例2
本实施例2所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆70份、富铝尖晶石11份、焦宝石18份、刚玉粉8份、碱式碳酸镁3份、单质硅12份、氧化钛1.2份、氧化硼3份、氧化钇1.2份、添加剂1份、分散剂3.5份和结合剂12份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2为99％，余量为杂质。
富铝尖晶石中Al2O3的质量含量为88wt％。
焦宝石的化学组成为：Al2O346％、SiO2 52％、Fe2O31.0％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈35％、聚乙二醇30％和羧甲基丙烯酰胺35％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇40％、亚甲基双丙烯酰胺30％和钼酚醛树脂30％。
添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物。
聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.5:1。
本实施例2所述的氧化锆耐火材料的制备方法，由以下步骤组成：
(1)将电熔单斜氧化锆、富铝尖晶石和焦宝石粉碎至0.025mm；
(2)将电熔单斜氧化锆、富铝尖晶石、焦宝石、刚玉粉、碱式碳酸镁、单质硅、氧化钛、氧化硼、氧化钇与分散剂混合均匀，得到预混料；
(3)将预混料与结合剂搅拌混合，并放入模具中压制形成坯体，坯体于850℃下烘干；
(4)将烘干后的坯体浸渍添加剂溶液，于200℃进行固化，然后于烧结炉中进行高温烧结，冷却至室温，制备得到氧化锆耐火材料。
其中：
步骤(3)中所述的压制成型为首先进行干压成型，然后进行冷等静压成型，干压成型压力为55Mpa，保压时间为25s，然后进行冷等静压成型，压强为35MPa，保压时间为70s。
步骤(4)中所述于1800℃煅烧2.8h进行高温烧结。
对实施例2制备的氧化锆耐火材料进行性能测试，1800℃下热膨胀率为0.43％，常温耐压为464MPa。
实施例3
本实施例3所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆65份、富铝尖晶石10份、焦宝石15份、刚玉粉5份、碱式碳酸镁2.8份、单质硅10份、氧化钛1.0份、氧化硼2.5份、氧化钇1份、添加剂0.9份、分散剂2.5份和结合剂5份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2为99％，余量为杂质。
富铝尖晶石中Al2O3的质量含量为88wt％。
焦宝石的化学组成为：Al2O346％、SiO2 52％、Fe2O31.0％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈33％、聚乙二醇30％和羧甲基丙烯酰胺37％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇40％、亚甲基双丙烯酰胺35％和钼酚醛树脂25％。
添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物。
聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.4:1。
本实施例3所述的氧化锆耐火材料的制备方法，由以下步骤组成：
(1)将电熔单斜氧化锆、富铝尖晶石和焦宝石粉碎至0.03mm；
(2)将电熔单斜氧化锆、富铝尖晶石、焦宝石、刚玉粉、碱式碳酸镁、单质硅、氧化钛、氧化硼、氧化钇与分散剂混合均匀，得到预混料；
(3)将预混料与结合剂搅拌混合，并放入模具中压制形成坯体，坯体于800℃下烘干；
(4)将烘干后的坯体浸渍添加剂溶液，于190℃进行固化，然后于烧结炉中进行高温烧结，冷却至室温，制备得到氧化锆耐火材料。
其中：
步骤(3)中所述的压制成型为首先进行干压成型，然后进行冷等静压成型，干压成型压力为50Mpa，保压时间为30s，然后进行冷等静压成型，压强为30MPa，保压时间为80s。
步骤(4)中所述于1750℃煅烧3h进行高温烧结。
对实施例3制备的氧化锆耐火材料进行性能测试，1800℃下热膨胀率为0.67％，常温耐压为405MPa。
对比例1
本对比例1所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆70份、富铝尖晶石11份、焦宝石18份、刚玉粉8份、碱式碳酸镁3份、单质硅12份、氧化钛1.2份、氧化硼3份、氧化钇1.2份、分散剂3.5份和结合剂12份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2为99％，余量为杂质。
富铝尖晶石中Al2O3的质量含量为88wt％。
焦宝石的化学组成为：Al2O346％、SiO2 52％、Fe2O31.0％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈35％、聚乙二醇35％和羧甲基丙烯酰胺40％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇40％、亚甲基双丙烯酰胺30％和钼酚醛树脂30％。
本对比例1所述的氧化锆耐火材料的制备方法与实施例2相同。
对对比例1制备的氧化锆耐火材料进行性能测试，1800℃下热膨胀率为0.98％，常温耐压为365MPa。
对比例2
本实施例2所述的氧化锆耐火材料，以重量份数计，原料组成如下：电熔单斜氧化锆70份、焦宝石18份、刚玉粉15份、碱式碳酸镁3份、单质硅12份、氧化钛1.2份、氧化硼3份、氧化钇1.2份、添加剂1份、分散剂3.5份和结合剂12份。
其中：
电熔单斜氧化锆的化学组成为：ZrO2为99％，余量为杂质。
焦宝石的化学组成为：Al2O346％、SiO2 52％、Fe2O31.0％、余量为杂质。
分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈35％、聚乙二醇35％和羧甲基丙烯酰胺40％。
结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇40％、亚甲基双丙烯酰胺30％和钼酚醛树脂30％。
添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物。
聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.5:1。
本对比例2所述的制备方法与实施例2相同。
对对比例2制备的氧化锆耐火材料进行性能测试，1800℃下热膨胀率为1.32％，常温耐压为332MPa。

Claims (8)

1.一种氧化锆耐火材料，其特征在于：以重量份数计，原料组成如下：电熔单斜氧化锆65-70份、富铝尖晶石10-12份、焦宝石15-18份、刚玉粉5-8份、碱式碳酸镁2.5-3.0份、单质硅8-12份、氧化钛0.8-1.2份、氧化硼2-3份、氧化钇0.8-1.2份、添加剂0.8-1.0份、分散剂2.5-3.5份和结合剂5-12份；
其中：所述的添加剂为聚碳锆烷溶液与聚四氟乙烯分散液的混合物，聚碳锆烷溶液与聚四氟乙烯分散液的质量比为1.5-1.3:1。
2.根据权利要求1所述的氧化锆耐火材料，其特征在于：电熔单斜氧化锆的化学组成为：ZrO2≥99%，余量为杂质；富铝尖晶石中Al2O3的质量含量＞85wt%；焦宝石的化学组成为：Al2O3 45-46%、SiO2 51-53%、Fe2O3 0.8-1.2%、余量为杂质。
3.根据权利要求1所述的氧化锆耐火材料，其特征在于：分散剂为聚丙烯腈、聚乙二醇和羧甲基丙烯酰胺的混合物。
4.根据权利要求3所述的氧化锆耐火材料，其特征在于：以质量百分数计，所述的分散剂由以下原料组成：聚丙烯腈30-35%、聚乙二醇30-35%和羧甲基丙烯酰胺35-40%。
5.根据权利要求1所述的氧化锆耐火材料，其特征在于：结合剂为聚乙烯醇、亚甲基双丙烯酰胺和钼酚醛树脂混合物。
6.根据权利要求5所述的氧化锆耐火材料，其特征在于：以质量百分数计，所述的结合剂由以下原料组成：聚乙二醇35-45%、亚甲基双丙烯酰胺25-35%和钼酚醛树脂25-35%。
7.一种权利要求1所述的氧化锆耐火材料的制备方法，其特征在于：由以下步骤组成：
（1）将电熔单斜氧化锆、富铝尖晶石和焦宝石粉碎至0.025-0.03mm；
（2）将电熔单斜氧化锆、富铝尖晶石、焦宝石、刚玉粉、碱式碳酸镁、单质硅、氧化钛、氧化硼、氧化钇与分散剂混合均匀，得到预混料；
（3）将预混料与结合剂搅拌混合，并放入模具中压制形成坯体，坯体于750-850℃下烘干；
（4）将烘干后的坯体浸渍添加剂溶液，于180-200℃进行固化，然后于烧结炉中进行高温烧结，冷却至室温，制备得到氧化锆耐火材料。
8.根据权利要求7所述的氧化锆耐火材料的制备方法，其特征在于：
步骤（3）中所述的压制成型为首先进行干压成型，然后进行冷等静压成型，干压成型压力为50-55 MPa，保压时间为25-35s，然后进行冷等静压成型，压强为30-35MPa，保压时间为60-80s；
步骤（4）中所述于1750-1850℃煅烧2.5-3h进行高温烧结。
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