CN116332635B - 一种电熔锆镁铬尖晶石原料及其制备方法 - Google Patents
一种电熔锆镁铬尖晶石原料及其制备方法 Download PDFInfo
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 66
- 239000011029 spinel Substances 0.000 title claims abstract description 66
- 239000002994 raw material Substances 0.000 title claims abstract description 61
- 238000003723 Smelting Methods 0.000 title claims abstract description 36
- BFXREAXRMUFNRP-UHFFFAOYSA-N [Mg][Zr][Cr] Chemical compound [Mg][Zr][Cr] BFXREAXRMUFNRP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 74
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 50
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 47
- 239000011651 chromium Substances 0.000 claims abstract description 20
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 19
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 19
- NACUKFIFISCLOQ-UHFFFAOYSA-N [Mg].[Cr] Chemical compound [Mg].[Cr] NACUKFIFISCLOQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 19
- 229910052804 chromium Inorganic materials 0.000 claims description 13
- 239000011449 brick Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000008859 change Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000005065 mining Methods 0.000 abstract description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052726 zirconium Inorganic materials 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- NJFMNPFATSYWHB-UHFFFAOYSA-N ac1l9hgr Chemical compound [Fe].[Fe] NJFMNPFATSYWHB-UHFFFAOYSA-N 0.000 description 1
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- UOUJSJZBMCDAEU-UHFFFAOYSA-N chromium(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[Cr+3].[Cr+3] UOUJSJZBMCDAEU-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- MHKWSJBPFXBFMX-UHFFFAOYSA-N iron magnesium Chemical compound [Mg].[Fe] MHKWSJBPFXBFMX-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
本发明公开了一种电熔锆镁铬尖晶石原料及其制备方法,这种电熔锆镁铬尖晶石原料的化学成分含量为Cr2O3 70‑95wt%,MgO 3‑23wt%,ZrO2 2‑7wt%,主要晶相为锆镁铬尖晶石;将氧化铬原料与氧化镁、氧化锆混合后,在矿冶炉内熔炼,熔炼温度为1800℃以上,熔炼完成后,经冷却破粉碎后,合成一种新型的致密电熔含锆镁铬尖晶石原料,这种电熔锆镁铬尖晶石原料的吸水率低,体积密度大,氧化锆在高温下的相变转化能明显改善其韧性,提高尖晶石材料柔韧度。
Description
技术领域
本发明涉及耐火材料技术领域,尤其涉及一种电熔锆镁铬尖晶石原料及其制备方法。
镁铬尖晶石是一种优良的耐火原料,但是镁铬尖晶石在自然界中多以铬铁矿形式存在,极少独自存在。由于铬铁矿含有镁、铬、铝、铁四种氧化物,其矿相是镁铬尖晶石、镁铝尖晶石、镁铁尖晶石、铁铝尖晶石、铁铬尖晶石和铁铁尖晶石的复合体,另外铬铁矿中镁铬尖晶石含量也较低,限制了镁铬尖晶石性能的发挥。当前市场上的镁铬熔块多是以氧化镁和铬铁矿为主要原料制备的,Cr2O3含量在20%左右,还有较多的MgO、FeOn、Al2O3和其它少量杂质。
镁铬尖晶石的合成方法较多,耐火材料应用一般为烧结法或电熔法。烧结法合成镁铬尖晶石时,由于氧化铬的蒸发凝聚作用,导致合成的镁铬尖晶石多为带孔的疏松体,孔隙率高,积密度较低,难以在耐火材料中大量应用。电熔法合成的镁铬尖晶石则能达到致密结构,在耐火材料中能广泛应用,且镁铬尖晶石近似于化学计量的镁铬尖晶石。
本发明主要合成Cr2O3含量大于70%的锆镁铬尖晶石,锆镁铬尖晶石矿相设计为镁铬尖晶石、氧化锆及氧化铬,制备一种新的电熔含锆镁铬尖晶石原料,提高尖晶石材料柔韧度。
发明内容
针对以上问题,本发明提供一种电熔锆镁铬尖晶石原料及其制备方法,以氧化铬原料、氧化镁、氧化锆为主要原料,经混合后在电炉中合成一种新型的致密电熔含锆镁铬尖晶石原料,由于含锆镁铬尖晶石原料中主晶相为镁铬尖晶石,镁铬尖晶石是一种优良的耐火高温原料,另外还含有氧化锆,氧化锆在高温下的相变转化可能明显改善其韧性,提高材料柔韧度。
本发明为实现上述目的所采用的技术方案为一种电熔锆镁铬尖晶石原料,其化学成分含量为:Cr2O3为70-95wt%,MgO为18-23wt%,ZrO2为2-7wt%;原始料包括氧化铬原料、氧化镁、氧化锆。
一种电熔锆镁铬尖晶石原料的制备方法为:
步骤一、原始料加入的重量份数分别为:氧化铬原料70-95份,氧化镁18-23份,氧化锆2-7份;
步骤二、氧化铬原料经加工拣选后,将氧化铬粗粉、氧化镁粉和氧化锆粉混合后,在电炉内熔炼,熔炼温度为1800℃以上,熔炼完成后,经冷却破粉碎后,得到这种电熔锆镁铬尖晶石原料。
其中氧化铬原料为氧化铬粗粉或高铬残砖;氧化铬原料为氧化铬粗粉时,氧化铬的粒度<10mm的颗粒重量份数占95%以上;氧化铬原料为高铬残砖时,高铬残砖的粒度<3mm的颗粒重量份数占95%以上。
其中氧化镁粉的粒度小于1mm,氧化锆的粒度小于0.045mm。
得到的这种电熔锆镁铬尖晶石原料,主要晶相为镁铬尖晶石,次晶相为氧化铬、氧化锆。
得到这种电熔锆镁铬尖晶石原料,生成的晶相为:镁铬尖晶石70-90%,氧化铬5-20%,斜锆石0-7%。
其中氧化铬原料经加工后,粒度<3mm的颗粒占95%以上,氧化镁粉的粒度小于1mm,氧化锆的粒度小于0.045mm。在后续的工艺中氧化镁和氧化铬反应生成镁铬尖晶石,氧化镁完全生成尖晶石,多余的氧化铬则生成氧化铬晶体,氧化锆则镶嵌在镁铬尖晶石和氧化铬的晶须之间,起到栅栏作用,在高温下利用其相变机理能提高材料的韧性。
其中氧化铬原料为氧化铬粗粉时,其中的Cr2O3含量大于98wt%;氧化铬原料为高铬残砖时,其中的Cr2O3含量大于80wt%,ZrO2含量为2-7wt%;氧化镁中MgO的含量大于85wt%;氧化锆中ZrO2的含量大于95wt%。
其中氧化铬与氧化镁和氧化锆的重量配比最优为77︰18︰5,由于镁铬尖晶石中Cr2O3的含量为79wt%,MgO的含量21%,为了原料中氧化镁全部转化为镁铬尖晶石,所以配比中氧化镁的含量稍低于理论值,这样合成的尖晶石原料中其矿物相应为反应生成的镁铬尖晶石,未反应完全的铬氧化物,以及添加的氧化锆。考虑到MgO和Cr2O3反应后生成的镁铬尖晶石在高温下是一固溶体(见图1),所以原料配比中氧化铬和氧化镁的化学含量大于79︰21的范围内。
有益效果:本发明创新地在镁铬尖晶石中引入氧化锆,以氧化铬原料、氧化镁、氧化锆为主要原料,经混合后在电炉中合成一种新型的致密电熔含锆镁铬尖晶石原料,主晶相为镁铬尖晶石,利用氧化锆的相变机理,氧化锆在高温下的相变转化可能明显改善其韧性,提高尖晶石材料柔韧度。
该电熔锆镁铬尖晶石料的物理性能典型值为:吸水率1.0%,体积密度4.34g/cm3,镁铬尖晶石固溶体85-90%左右,铬氧化物5-10%左右,氧化锆5%左右。
附图说明
图1为本发明MgO和Cr2O3系相图;
图2为本发明电熔锆镁铬尖晶石的XRD图。
实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例,并不能因此而理解为对本发明专利范围的限制。基于本发明中的实施例,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。
参照以下实施例可以对本发明作进一步详细说明,但本发明并不局限于这些实施例。
实施例
一种电熔锆镁铬尖晶石原料的制备方法为:
步骤一、原始料包括氧化铬粗粉、高纯镁砂、氧化锆,加入的重量份数分别为:氧化铬粗粉77份,高纯镁砂18份,氧化锆5份;
步骤二、氧化铬粗粉的粒度为10-0mm的通料,高纯镁砂的粒度为1-0mm的通料,与氧化锆粉混合后,在矿冶炉内熔炼,熔炼温度为1800℃以上,熔炼完成后,经冷却破粉碎后,得到这种电熔锆镁铬尖晶石原料。
得到的这种电熔锆镁铬尖晶石原料,其化学成分中氧化铬和氧化镁的含量合量为93.56wt%,氧化锆为4.32wt%,气孔率1.5%,体积密度3.34%。
生成的晶相为:镁铬尖晶石85-90%,铬氧化物5%,斜锆石为0-5%。
实施例
一种电熔锆镁铬尖晶石原料的制备方法为:
步骤一、原始料包括高铬残砖、轻烧氧化镁,加入的重量份数分别为:高铬残砖80份,轻烧氧化镁20份;
步骤二、高铬残砖经拣选后,破碎为3-0mm的通料,轻烧氧化镁粒度为1-0mm的通料,经混合后,在矿冶炉内熔炼,熔炼温度为 1800℃以上,熔炼完成后,经冷却破粉碎后,得到这种电熔锆镁铬尖晶石原料。
得到的这种电熔锆镁铬尖晶石原料,其化学成分中氧化铬和氧化镁的含量合量为92.78wt%,氧化锆为2.68wt%,气孔率1.6%,体积密度3.32%。
生成的晶相为:镁铬尖晶石85-90%,铬氧化物5-10%,斜锆石0-5%。
Claims (6)
1.一种电熔锆镁铬尖晶石原料,其特征在于:电熔锆镁铬尖晶石原料的化学成分及含量为:Cr2O3 70-95wt%,MgO 18-23wt%,ZrO2 2-7wt%;原始料包括氧化铬原料、氧化镁和氧化锆,得到这种电熔锆镁铬尖晶石原料的主晶相为镁铬尖晶石,次晶相为氧化铬、氧化锆。
2.根据权利要求1所述的一种电熔锆镁铬尖晶石原料,其特征在于:氧化铬原料为氧化铬粗粉或高铬残砖;氧化铬原料为氧化铬粗粉时,氧化铬中的Cr2O3含量大于98wt%,氧化铬的粒度<10mm的颗粒重量份数占95%以上;氧化铬原料为高铬残砖时,高铬残砖的粒度<3mm的颗粒重量份数占95%以上;高铬残砖中的Cr2O3含量大于80wt%,ZrO2含量为2-7wt%。
3.根据权利要求1所述的一种电熔锆镁铬尖晶石原料,其特征在于:氧化镁为高纯镁砂、烧结镁砂、轻烧镁粉中的一种或以上,氧化镁原料中MgO的含量大于85wt%,粒度小于1mm;氧化锆原料中ZrO2的含量大于95 wt%,氧化锆微粉的粒度小于0.045mm。
4.根据权利要求1所述的一种电熔锆镁铬尖晶石原料的制备方法,其特征在于:氧化铬与氧化镁、氧化锆的重量配比最优为77:18:5。
5.根据权利要求1所述的一种电熔锆镁铬尖晶石原料,其特征在于:锆镁铬尖晶石中,镁铬尖晶石70-90%,氧化铬5-20%,斜锆石5-7%。
6.根据权利要求1所述的一种电熔锆镁铬尖晶石原料的制备方法,其特征在于:
步骤一、原始料加入的重量份数为:氧化铬原料70-95份,氧化镁18-23份,氧化锆2-7份;
步骤二、氧化铬原料经加工拣选后,将氧化铬原料、氧化镁粉和氧化锆粉混合后,在电炉内熔炼,熔炼温度为1800℃以上,熔炼完成后,经冷却破粉碎后,得到这种电熔锆镁铬尖晶石原料。
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