CN116462519A - 一种氢冶金用刚玉质耐火材料及其制备方法 - Google Patents
一种氢冶金用刚玉质耐火材料及其制备方法 Download PDFInfo
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- 239000010431 corundum Substances 0.000 title claims abstract description 80
- 239000011819 refractory material Substances 0.000 title claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 41
- 239000001257 hydrogen Substances 0.000 title claims abstract description 41
- 238000005272 metallurgy Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 12
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
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- 239000000843 powder Substances 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000004408 titanium dioxide Substances 0.000 claims description 12
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
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- 239000010936 titanium Substances 0.000 description 4
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
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- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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Abstract
本发明公开了一种氢冶金用刚玉质耐火材料及其制备方法。制备方法以70~85wt%的板状刚玉、8~15wt%的铝酸钙水泥、0.5~9wt%的钛白粉和2~7wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、干燥,制得刚玉预制块,再将刚玉预制块经过埋碳条件保温一段时间得到氢冶金用刚玉质耐火材料。本发明制备的氢冶金用刚玉质耐火材料高温强度大、热震稳定性好、抗H2‑H2O气体腐蚀性能强,适用于采用H2或H2+CO混合气为还原剂的氢冶金高温工业炉。
Description
技术领域
本发明涉及耐火材料技术领域,尤其涉及一种氢冶金用刚玉质耐火材料及其制备方法。
背景技术
氢冶金是采用氢气部分取代或完全取代碳作为铁矿石的还原剂,在低于铁熔点的温度范围内得到固态含铁料的技术。高纯H2在800℃下保温6小时,能够将铁矿石完全还原成Fe。高温下H2具有极强的还原性,同时H2还原铁矿石形成大量H2O(g),高温下的H2-H2O(g)混合气体对炉衬耐火材料提出了新的要求。
刚玉是目前应用最为广泛的耐火原料,具有优良的高温性能和化学稳定性,不易被H2-H2O(g)混合气体腐蚀。然而,刚玉砖的热震稳定性有待提高;另外,为提高抗H2-H2O(g)腐蚀性能,要求刚玉砖纯度高,这会导致烧结较为困难,高温结合强度不足。董伟霞等人(董伟霞,顾幸勇,李鑫浩,等.耐火材料,2016,50(6):416-419.)以煤矸石、氢氧化铝为主要原料,外加3%的金属氧化物(V2O5、MnO2或MgO)添加剂,于1500℃保温1h煅烧后制备了莫来石晶须增强刚玉耐火材料,原位生成的莫来石补强了刚玉基体;周秀丽等人(周秀丽,黄海,马北越,等.工业加热,2014,43(4):49-51.)在刚玉砖中添加ZrO2-SiC复合粉及工业SiC粉大幅提高材料热震稳定性;一种高炉陶瓷杯用Al2OC-AlN固溶体结合刚玉耐火材料及制备方法(CN202011009925.4)以刚玉为主要原料,酚醛树脂为结合剂,添加Al,经过高温N2下烧成,原位生成Al2OC-AlN固溶体结合相,常温耐压强度高达260-340MPa。然而,莫来石易被H2还原造成损毁,SiC、Al2OC-AlN等非氧化结合相易被高温H2O(g)腐蚀。所以,进一步提高刚玉砖的热震稳定性和高温结合强度,同时降低显气孔率减少H2-H2O(g)混合气体的渗透是其在氢冶金用炉衬耐火材料中成功使用的前提与关键。
发明内容
本发明的目的在于,针对现有技术的上述不足,提出一种高温强度大、热震稳定性好、抗H2-H2O气体腐蚀性能强的氢冶金用刚玉质耐火材料及其制备方法。
本发明的一种氢冶金用刚玉质耐火材料的制备方法,以70~85wt%的板状刚玉、8~15wt%的铝酸钙水泥、0.5~9wt%的钛白粉和2~7wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、干燥,制得刚玉预制块,再将刚玉预制块经过埋碳条件保温一段时间得到氢冶金用刚玉质耐火材料。
进一步的,将所述刚玉预制块经过1600℃~1800℃埋碳条件保温3~8h得到氢冶金用刚玉质耐火材料。
进一步的,干燥的温度为100~200℃。
进一步的,所述板状刚玉的Al2O3含量≥98wt%;所述板状刚玉的颗粒级配是:
粒径小于5mm且大于等于3mm占板状刚玉30~40wt%;
粒径小于3mm且大于等于1mm占板状刚玉40~55wt%;
粒径小于0.088mm占板状刚玉10~22wt%。
进一步的,所述铝酸钙水泥的CaO≥29.6wt%;Al2O3≥69.3wt%,所述铝酸钙水泥的中位径为11.34μm。
进一步的,所述钛白粉的TiO2≥98wt%,所述钛白粉的粒径≤0.074mm。
进一步的,所述氧化铝微粉的Al2O3含量≥99wt%,所述氧化铝微粉的中位径为2μm。
进一步的,所述减水剂为聚醚、聚羧酸、三聚磷酸钠、四聚磷酸钠和六偏磷酸钠中的任一种或两种的混合物。
进一步的,所述减水剂的质量为原料质量的0.1%-0.8%。
一种氢冶金用刚玉质耐火材料,采用上述的制备方法制备的氢冶金用刚玉质耐火材料。
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:
以板状刚玉为主要原料,添加8~15wt%的铝酸钙水泥结合剂,高温烧成过程中能够原位生成六铝酸钙(CaAl12O19,简写为CA6)结合相,大幅提高刚玉质耐火材料的结合强度。同时总压为1个大气压下,CA6与H2反应产物平衡分压由式(1)和(2)决定:
CaAl12O19 (s)+H2 (g)=Ca (g)+H2O (g)+6Al2O3 (1)
表1不同温度下六铝酸钙与氢气反应气体产物的平衡分压
不同温度下气体产物分压由(2)计算,结果如表1所示,可以看出即使升温至1800℃,气体产物平衡分压仅为1.62Pa,CA6在高纯H2条件下表现出优异的化学稳定性。原位生成CA6结合相不仅能提高刚玉质耐火材料结合相,同时具有优良的抗高温H2-H2O气体腐蚀性能。此外,针对CA6难以烧结致密化的问题,本方案通过添加钛白粉,在埋碳条件下烧成,埋碳条件下TiO2易被还原生成Ti3O5,即部分Ti4+被还原生成Ti3+,Ti3+易固溶于CA6中,形成固溶体,促进CA6烧结致密化,进而降低刚玉质耐火材料的显气孔率,阻碍高温下H2-H2O气体向材料内部渗透。
本发明制备的氢冶金用刚玉质耐火材料经过检测:显气孔率为12~18%;高温抗折强度为15~25MPa;常温抗折强度为20~35MPa;热震(首先加热到1100℃保温30min,然后放入流动水中冷却)循环5次后残余抗折强度为10~25MPa;经过900℃下的H2-H2O混合气体腐蚀10h后,常温抗折强度为14~29MPa。
因此,本发明制备的氢冶金用刚玉质耐火材料高温强度大、热震稳定性好、抗H2-H2O气体腐蚀性能强,适用于采用H2或H2+CO混合气为还原剂的氢冶金高温工业炉。
具体实施方式
以下是本发明的具体实施例,对本发明的技术方案作进一步的描述,但本发明并不限于这些实施例。
实施例1
一种氢冶金用刚玉质耐火材料及其制备方法。本实施例所述制备方法是:
以70~75wt%的板状刚玉、13~15wt%的铝酸钙水泥、6~9wt%的钛白粉和4~7wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、110℃干燥,制得刚玉预制块,再经过1600℃~1800℃埋碳条件保温3h得到氢冶金用刚玉质耐火材料。
本实施例制备的氢冶金用刚玉质耐火材料经过检测:显气孔率为12~17%;高温抗折强度为17~23MPa;常温抗折强度为28~32MPa;热震(首先加热到1100℃保温30min,然后放入流动水中冷却)循环5次后残余抗折强度为23~28MPa;经过900℃下的H2-H2O混合气体腐蚀10h后,常温抗折强度为25~28MPa。
实施例2
一种氢冶金用刚玉质耐火材料及其制备方法。本实施例所述制备方法是:
以74~80wt%的板状刚玉、11~14wt%的铝酸钙水泥、4~7wt%的钛白粉和3~6wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、110℃干燥,制得刚玉预制块,再经过1600℃~1800℃埋碳条件保温3h得到氢冶金用刚玉质耐火材料。
本实施例制备的氢冶金用刚玉质耐火材料经过检测:显气孔率为12~16%;高温抗折强度为20~25MPa;常温抗折强度为30~35MPa;热震(首先加热到1100℃保温30min,然后放入流动水中冷却)循环5次后残余抗折强度为20~25MPa;经过900℃下的H2-H2O混合气体腐蚀10h后,常温抗折强度为24~29MPa。
实施例3
一种氢冶金用刚玉质耐火材料及其制备方法。本实施例所述制备方法是:
以79~83wt%的板状刚玉、10~13wt%的铝酸钙水泥、2~5wt%的钛白粉和2~4wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、110℃干燥,制得刚玉预制块,再经过1600℃~1800℃埋碳条件保温3h得到氢冶金用刚玉质耐火材料。
本实施例制备的氢冶金用刚玉质耐火材料经过检测:显气孔率为15~18%;高温抗折强度为18~22MPa;常温抗折强度为25~29MPa;热震(首先加热到1100℃保温30min,然后放入流动水中冷却)循环5次后残余抗折强度为16~21MPa;经过900℃下的H2-H2O混合气体腐蚀10h后,常温抗折强度为17~25MPa。
实施例4
一种氢冶金用刚玉质耐火材料及其制备方法。本实施例所述制备方法是:
以82~85wt%的板状刚玉、8~12wt%的铝酸钙水泥、0.5~3.5wt%的钛白粉和2~4wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、110℃干燥,制得刚玉预制块,再经过1600℃~1800℃埋碳条件保温3h得到氢冶金用刚玉质耐火材料。
本实施例制备的氢冶金用刚玉质耐火材料经过检测:显气孔率为16~18%;高温抗折强度为15~19MPa;常温抗折强度为20~26MPa;热震(首先加热到1100℃保温30min,然后放入流动水中冷却)循环5次后残余抗折强度为10~17MPa;经过900℃下的H2-H2O混合气体腐蚀10h后,常温抗折强度为11~18MPa。
以上未涉及之处,适用于现有技术。
虽然已经通过示例对本发明的一些特定实施例进行了详细说明,但是本领域的技术人员应该理解,以上示例仅是为了进行说明,而不是为了限制本发明的范围,本发明所属技术领域的技术人员可以对所描述的具体实施例来做出各种各样的修改或补充或采用类似的方式替代,但并不会偏离本发明的方向或者超越所附权利要求书所定义的范围。本领域的技术人员应该理解,凡是依据本发明的技术实质对以上实施方式所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围。
Claims (10)
1.一种氢冶金用刚玉质耐火材料的制备方法,其特征在于:以70~85wt%的板状刚玉、8~15wt%的铝酸钙水泥、0.5~9wt%的钛白粉和2~7wt%的氧化铝微粉为原料,加入减水剂,混合均匀,得到预混料;向预混料中加入水,搅拌均匀,浇注成型,经过室温养护、脱模、干燥,制得刚玉预制块,再将刚玉预制块经过埋碳条件保温一段时间得到氢冶金用刚玉质耐火材料。
2.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:将所述刚玉预制块经过1600℃~1800℃埋碳条件保温3~8h得到氢冶金用刚玉质耐火材料。
3.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:干燥的温度为100~200℃。
4.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述板状刚玉的Al2O3含量≥98wt%;所述板状刚玉的颗粒级配是:
粒径小于5mm且大于等于3mm占板状刚玉30~40wt%;
粒径小于3mm且大于等于1mm占板状刚玉40~55wt%;
粒径小于0.088mm占板状刚玉10~22wt%。
5.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述铝酸钙水泥的CaO≥29.6wt%;Al2O3≥69.3wt%,所述铝酸钙水泥的中位径为11.34μm。
6.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述钛白粉的TiO2≥98wt%,所述钛白粉的粒径≤0.074mm。
7.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述氧化铝微粉的Al2O3含量≥99wt%,所述氧化铝微粉的中位径为2μm。
8.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述减水剂为聚醚、聚羧酸、三聚磷酸钠、四聚磷酸钠和六偏磷酸钠中的任一种或两种的混合物。
9.根据权利要求1所述的氢冶金用刚玉质耐火材料的制备方法,其特征在于:所述减水剂的质量为原料质量的0.1%-0.8%。
10.一种氢冶金用刚玉质耐火材料,其特征在于:采用权利要求1-9任一项所述的制备方法制备的氢冶金用刚玉质耐火材料。
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