CN118125845A - 一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法 - Google Patents
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法 Download PDFInfo
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 53
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 62
- 238000001816 cooling Methods 0.000 claims abstract description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 54
- 239000000395 magnesium oxide Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 18
- 229910052596 spinel Inorganic materials 0.000 claims description 17
- 239000011029 spinel Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 22
- 229910052782 aluminium Inorganic materials 0.000 claims 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims 4
- 239000000203 mixture Substances 0.000 claims 3
- 238000010438 heat treatment Methods 0.000 claims 2
- 239000011812 mixed powder Substances 0.000 claims 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims 1
- 239000011258 core-shell material Substances 0.000 claims 1
- 238000003825 pressing Methods 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 25
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 13
- 230000003628 erosive effect Effects 0.000 abstract description 11
- 229960004887 ferric hydroxide Drugs 0.000 abstract description 11
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 abstract description 11
- 230000035939 shock Effects 0.000 abstract description 11
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 7
- 238000004806 packaging method and process Methods 0.000 abstract description 7
- 238000012216 screening Methods 0.000 abstract description 7
- 235000012245 magnesium oxide Nutrition 0.000 description 24
- 239000011148 porous material Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000011777 magnesium Substances 0.000 description 8
- 238000000465 moulding Methods 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 6
- 239000002893 slag Substances 0.000 description 6
- 239000001095 magnesium carbonate Substances 0.000 description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 5
- 235000014380 magnesium carbonate Nutrition 0.000 description 5
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000013081 microcrystal Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910001691 hercynite Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
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Abstract
本发明具体涉及一种基于氢氧化镁的轻量MgO‑MgFe2O4骨料及其制备方法。其特征在于以85.0～97.0wt％的氢氧化镁细粉和3.0～15.0wt％的氧化铁细粉为原料，外加所述原料1.0～3.0wt％的氢氧化铁细粉和2.0～5.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1400～1600℃条件下保温1～4小时，冷却，破碎，筛分，包装，制得基于氢氧化镁的轻量MgO‑MgFe2O4骨料。本发明所制备的基于氢氧化镁的轻量MgO‑MgFe2O4骨料具有晶粒尺寸大、强度大、抗热震性能优异和抗侵蚀性能优良的特点。
Description
技术领域
本发明属于轻量镁砂技术领域。具体涉及一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。
背景技术
镁砂具有熔点高(约2800℃)及抗碱性渣性能优良的特性，是炼钢转炉、电炉、钢包和其他冶金炉炉衬广泛使用的一种耐火原料。近些年，为降低冶金炉炉衬热量耗散，实现冶金行业节能减排的目的，研究人员通过在镁砂中引入一定量的气孔，开发了低导热系数的轻量镁砂。
“一种轻量化方镁石-镁铁铝复合尖晶石耐火材料的制备方法”(CN111170724A)专利技术，以低品位菱镁矿为原料制备了轻量化方镁石-镁铁铝复合尖晶石骨料，该技术主要缺陷在于天然菱镁矿杂质含量较多，烧结过程方镁石晶间会形成低熔点相，显著降低镁砂的高温力学性能，增大了气孔合并及长大，大幅降低了镁砂的抗侵蚀性能。
“一种基于盐湖卤水的镁砂骨料及其制备方”(CN107954729A)专利技术，该技术以水氯镁石为原料，通过引入可溶性盐制备了高纯镁砂，但该技术开发的镁砂平均孔径大，抗渣侵蚀性能较差。
“一种具有微-纳米复合孔结构的烧结镁砂及其制备方法”(CN108821750A)专利技术，该技术以含镁原料微粉及可溶性镁溶液为原料制备了具有微-纳米复合孔结构的轻量镁砂，但该轻量镁砂晶粒较小，显气孔率较高，导致强度、抗侵蚀性能及抗热冲击性能难以满足使用要求。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种晶粒尺寸大、强度大、抗热震性能优异和抗侵蚀性能优良的基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。
为实现上述目的，本发明所采用的技术方案是：
以85.0～97.0wt％的氢氧化镁细粉和3.0～15.0wt％的氧化铁细粉为原料，外加所述原料1.0～3.0wt％的氢氧化铁细粉和2.0～5.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1400～1600℃条件下保温1～4小时，冷却，破碎，筛分，包装，制得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2含量＞99wt％，氢氧化镁细粉的粒度为200～800μm。
所述氧化铁细粉的纯度＞98％，氧化铁细粉的粒度＜45μm。
所述氢氧化铁细粉的纯度＞98％，氢氧化铁细粉的粒度＜10μm。
所述聚乙烯醇的PH值为5～8。
所述成型的方式为机压成型，机压成型的压强为5～15MPa。
所述干燥的温度为80～110℃，干燥的时间9～12小时。
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：
本发明采用粒度为200～800μm的氢氧化镁为主要原料，所述氢氧化镁在400℃左右原位分解能形成含大量微纳米气孔及MgO微晶的团聚体。同时，所采用的另一原料氢氧化铁细粉分解形成的Fe2O3粒径细小、活性很高，能扩散进入所述团聚体内并与MgO微晶反应形成MgFe2O4相，阻碍所述团聚体内气孔的合并长大及排出。
本发明添加的Fe2O3细粉会随着温度进一步升高与MgO反应在团聚体间形成致密的MgFe2O4相，促进方镁石晶粒生长，使得大量微孔封闭在MgO团聚体内，保证制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料的闭气孔率高及晶粒尺寸大。
本发明形成的MgFe2O4相强化了团聚体间的结合，同时MgFe2O4相及闭口气孔可以吸收热应力并促进基于氢氧化镁的轻量MgO-MgFe2O4骨料内裂纹发生偏转，赋予制品高的强度和优良的抗热震性能。
另外，本发明形成的MgFe2O4相提高了MgO团聚体间的致密性，增大了镁砂晶粒尺寸，且MgFe2O4相能与渗入的熔渣反应，在团聚体间生成高熔点及高粘度的物质，阻止熔渣的进一步渗透及侵蚀，所制制品抗侵蚀性能优良。
本发明所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为150～300μm，显气孔率为0.3～1.0％，闭气孔率为15.5～21.5％，平均孔径为0.10～0.25μm，抗折强度为150～185MPa，500℃下导热系数为1.5～5.5W/(m·k)，热震稳定性在900℃下水冷1次残余强度保持率为65～85％。
因此，本发明所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料具有晶粒尺寸大、强度大、抗热震性能优异和抗侵蚀性能优良的特点。
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：
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。本具体实施方式所述制备方法是：
以85.0～97.0wt％的氢氧化镁细粉和3.0～15.0wt％的氧化铁细粉为原料，外加所述原料1.0～3.0wt％的氢氧化铁细粉和2.0～5.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1400～1600℃条件下保温1～4小时，冷却，破碎，筛分，包装，制得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2含量＞99wt％。
所述氧化铁细粉的纯度＞98％。
所述氢氧化铁细粉的纯度＞98％。
所述聚乙烯醇的PH值为5～8。
所述成型的方式为机压成型，机压成型的压强为5～15MPa。
所述干燥的温度为80～110℃，干燥的时间为9～12小时。
本具体实施方式中：
所述成型的方式为机压成型；
所述氢氧化镁细粉的粒度为200～800μm；
所述氧化铁细粉粒度＜45μm；
所述氢氧化铁细粉的粒度＜10μm。
实施例中不再赘述。
实施例1
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。本实施例所述制备方法是：
以85.0wt％氢氧化镁细粉和15.0wt％的Fe2O3细粉为原料，外加所述原料1.0wt％的Fe(OH)3细粉和2.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1400℃条件下保温1小时，冷却、破碎、筛分、包装，即得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2为99.1wt％。
所述氧化铁细粉的纯度为98.2％。
所述氢氧化铁细粉的纯度为98.2％。
所述聚乙烯醇的PH值为5。
所述机压成型的压强为5MPa。
所述干燥的温度为80℃，干燥的时间为9小时。
本实施例所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为150μm，显气孔率为0.3％；闭气孔率为15.5％；平均孔径为0.25μm；抗折强度为150MPa；500℃下导热系数为5.5W/(m·k)；热震稳定性在900℃下水冷1次残余强度保持率为65％。
实施例2
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。本实施例所述制备方法是：
以97.0wt％氢氧化镁细粉和3.0wt％的Fe2O3细粉为原料，外加所述原料3.0wt％的Fe(OH)3细粉和5.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1600℃条件下保温4小时，冷却、破碎、筛分、包装，即得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2为99.3wt％。
所述氧化铁细粉的纯度为98.4％。
所述氢氧化铁细粉的纯度为98.4％。
所述聚乙烯醇的PH值为8。
所述机压成型的压强为15MPa。
所述干燥的温度为110℃，干燥的时间为12小时。
本实施例所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为300μm，显气孔率为1.0％；闭气孔率为21.5％；平均孔径为0.10μm；抗折强度为185MPa；500℃下导热系数为1.5W/(m·k)；热震稳定性在900℃下水冷1次残余强度保持率为85％。
实施例3
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。本实施例所述制备方法是：
以90.0wt％氢氧化镁细粉和10.0wt％的Fe2O3细粉为原料，外加所述原料2.0wt％的Fe(OH)3细粉和3.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1500℃条件下保温2小时，冷却、破碎、筛分、包装，即得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2为99.5wt％。
所述氧化铁细粉的纯度为98.6％。
所述氢氧化铁细粉的纯度为98.6％。
所述聚乙烯醇的PH值为7。
所述机压成型的压强为12MPa。
所述干燥的温度为100℃，干燥的时间为11小时。
本实施例所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为250μm，显气孔率为0.7％；闭气孔率为17.5％；平均孔径为0.20μm；抗折强度为165MPa；500℃下导热系数为2.8W/(m·k)；热震稳定性在900℃下水冷1次残余强度保持率为77％。
实施例4
一种基于氢氧化镁的轻量MgO-MgFe2O4骨料及其制备方法。其特征在于以93.0wt％氢氧化镁细粉和7.0wt％的Fe2O3细粉为原料，外加所述原料2.5wt％的Fe(OH)3细粉和4.0wt％的聚乙烯醇，搅拌均匀，成型，干燥；然后于1550℃条件下处理3小时，冷却、破碎、筛分、包装，即得基于氢氧化镁的轻量MgO-MgFe2O4骨料。
所述氢氧化镁细粉的Mg(OH)2为99.4wt％。
所述氧化铁细粉的纯度为98.3％。
所述氢氧化铁细粉的纯度为98.3％。
所述聚乙烯醇的PH值为6。
所述机压成型的压强为8MPa。
所述干燥的温度为90℃，干燥的时间为10小时。
本实施例所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为200μm，显气孔率为0.5％；闭气孔率为19.0％；平均孔径为0.15μm；抗折强度为178MPa；500℃下导热系数为3.6W/(m·k)，热震稳定性在900℃下水冷1次残余强度保持率为82％。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式采用粒度为200～800μm的氢氧化镁为主要原料，所述氢氧化镁在400℃左右原位分解能形成含大量微纳米气孔及MgO微晶的团聚体。同时，所采用的另一原料氢氧化铁细粉分解形成的Fe2O3粒径细小、活性很高，能扩散进入所述团聚体内并与MgO微晶反应形成MgFe2O4相，阻碍所述团聚体内气孔的合并长大及排出。
本具体实施方式添加的Fe2O3细粉会随着温度进一步升高与MgO反应在团聚体间形成致密的MgFe2O4相，促进方镁石晶粒生长，使得大量微孔封闭在MgO团聚体内，保证制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料的闭气孔率高及晶粒尺寸大。
本具体实施方式形成的MgFe2O4相强化了团聚体间的结合，同时MgFe2O4相及闭口气孔可以吸收热应力并促进基于氢氧化镁的轻量MgO-MgFe2O4骨料内裂纹发生偏转，赋予制品高的强度和优良的抗热震性能。
另外，本具体实施方式形成的MgFe2O4相提高了MgO团聚体间的致密性，增大了镁砂晶粒尺寸，且MgFe2O4相能与渗入的熔渣反应，在团聚体间生成高熔点及高粘度的物质，阻止熔渣的进一步渗透及侵蚀，所制制品抗侵蚀性能优良。
本具体实施方式所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料经检测：平均晶粒尺寸为150～300μm，显气孔率为0.3～1.0％，闭气孔率为15.5～21.5％，平均孔径为0.10～0.25μm，抗折强度为150～185MPa，500℃下导热系数为1.5～5.5W/(m·k)，热震稳定性在900℃下水冷1次残余强度保持率为65～85％。
因此，本具体实施方式所制备的基于氢氧化镁的轻量MgO-MgFe2O4骨料具有晶粒尺寸大、强度大、抗热震性能优异和抗侵蚀性能优良的特点。
Claims (8)
1.一种多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述制备方法的步骤是：
步骤一、以纳米氧化铝、α-氧化铝微粉和氢氧化铝微粉中的任意一种为铝源，或以纳米氧化铝、α-氧化铝微粉和氢氧化铝微粉中的任意两种的混合粉为铝源，或以纳米氧化铝、α-氧化铝微粉和氢氧化铝微粉三种的混合粉为铝源；
步骤二、将79～97wt％的氢氧化镁细粉和3～21wt％的所述铝源置于搅拌机内，外加所述氢氧化镁细粉和所述铝源之和4.5～5.5wt％的水，搅拌1～3h，得到混合料；
步骤三、将所述混合料在100～200MPa条件下机压成型，干燥；再以1～3℃/min的速率升温至300～400℃，保温0.5～1.5h；然后以2～5℃/min的速率升温至1600～1800℃，保温2～5h；随炉冷却，破碎，筛分，制得多微孔方镁石-镁铝尖晶石耐火骨料。
2.根据权利要求1所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述纳米氧化铝的粒径＜500nm；所述纳米氧化铝的Al2O3含量＞99wt％。
3.根据权利要求1所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述α-氧化铝微粉的粒径＜2μm；所述α-Al2O3微粉的Al2O3含量＞99wt％。
4.根据权利要求1所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述氢氧化铝微粉的粒径＜2μm；所述Al(OH)3微粉的Al2O3含量＞63wt％。
5.根据权利要求1所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述氢氧化镁细粉的粒径＜42μm；所述氢氧化镁细粉的MgO含量＞66wt％。
6.根据权利要求1所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法，其特征在于所述干燥：温度为90～110℃，时间为18～36h。
7.一种多微孔方镁石-镁铝尖晶石耐火骨料，其特征在于所述多微孔方镁石-镁铝尖晶石耐火骨料是根据权利要求1～6项中任一项所述的多微孔方镁石-镁铝尖晶石耐火骨料的制备方法所制备的多微孔方镁石-镁铝尖晶石耐火骨料。
8.根据权利要求7所述多微孔方镁石-镁铝尖晶石耐火骨料，其特征在于所述多微孔方镁石-镁铝尖晶石耐火骨料具有以含纳米孔的多孔氧化镁为核、以连续尖晶石为壳的微核壳结构；其中：多孔氧化镁的平均粒径为20～45μm，连续尖晶石壳的平均厚度为2.0～5.0μm。
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