CN114751729A - 一种氢冶金天然气基竖炉用硅砖及其制备方法 - Google Patents

一种氢冶金天然气基竖炉用硅砖及其制备方法 Download PDF

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CN114751729A
CN114751729A CN202210373926.XA CN202210373926A CN114751729A CN 114751729 A CN114751729 A CN 114751729A CN 202210373926 A CN202210373926 A CN 202210373926A CN 114751729 A CN114751729 A CN 114751729A
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shaft furnace
silicon
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顾华志
陈定
黄奥
张美杰
李少飞
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种氢冶金天然气基竖炉用硅砖及其制备方法。其技术方案是：以55～75wt％的硅石颗粒、16～30wt％的硅石细粉、3～7wt％的硅微粉、2～6wt％的石灰乳和1～6wt％的氧化钇为原料，混合，再外加所述原料1～5wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以15～45℃/h的速率升温至1350～1450℃，保温7～12h，制得氢冶金天然气基竖炉用硅砖。本发明制备的氢冶金天然气基竖炉用硅砖具有荷重软化点高、强度大、抗H2‑H2O气体腐蚀性能强和使用寿命长的特点，适用于采用H2或H2+CO混合气为还原剂的氢冶金天然气基竖炉制铁。

Description

一种氢冶金天然气基竖炉用硅砖及其制备方法
技术领域
本发明属于竖炉用硅砖技术领域。具体涉及一种氢冶金天然气基竖炉用硅砖及其制备方法。
背景技术
钢铁行业氢冶金就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。H2还原铁矿石工艺过程温度低、无温室气体排放，对于钢铁行业朝着节能减排、绿色制造的方向健康发展意义重大。与传统焦炭还原铁矿石相比，氢冶金用耐火材料的服役环境发生了巨大的变化，但H2还原铁矿石产生水蒸气，高温H2(g)和H2O(g)会对炉衬耐火材料服役性能产生巨大影响。
硅砖具有荷重软化点高、高温下体积膨胀性小、耐酸性渣的特点被用于氢冶金用天然气基竖炉。在硅砖制备过程中为了促进鳞石英的生成普遍需要添加矿化剂：张志豪等人(张志豪，张玲，关岩，等.冶金能源，2018，37(3)：47-50)采用复合矿化剂FeO、Ca(OH)2和MnO2，促进硅砖烧成过程中鳞石英的生成；肖伟等人(肖伟,曹梅,陈艳.耐火材料,2012,46(5):361-362.)以铁鳞和石灰乳作为矿化剂，制备了含鳞石英高达65wt％的硅砖；“一种硅砖及其制备方法”(CN102167606A)专利技术，以FeO和石灰乳的混合物为矿化剂，制备了荷重软化温度高达1692℃的硅砖。从以上技术可以看出，目前硅砖生产过程中使用的矿化剂主要包含CaO和FeO。而氢冶金生产过程中含有大量H2(g)和H2O(g)，矿化剂中的CaO易与H2O(g)反应产生体积膨胀造成硅砖损毁；FeO易被H2还原成Fe造成硅砖结构破坏。硅砖生产过程中引入的矿化剂抗H2-H2O气体腐蚀性能差，导致硅砖服役过程中产生结构破坏，不利于氢冶金用硅砖长寿化。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种氢冶金天然气基竖炉用硅砖的制备方法，用该方法制备的氢冶金天然气基竖炉用硅砖荷重软化点高、强度大、抗H2-H2O气体腐蚀性能强和使用寿命长。
为实现上述目的，本发明采用的技术方案是：以55～75wt％的硅石颗粒、16～30wt％的硅石细粉、3～7wt％的硅微粉、2～6wt％的石灰乳和1～6wt％的氧化钇为原料，混合，再外加所述原料1～5wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以15～45℃/h的速率升温至1350～1450℃，保温7～12h，制得氢冶金天然气基竖炉用硅砖。
所述硅石颗粒的SiO2含量≥98wt％；所述硅石颗粒的级配是：粒径小于5mm且大于等于3mm占硅石颗粒20～30wt％，粒径小于3mm且大于等于1mm占硅石颗粒40～55wt％，粒径小于1mm且大于等于0.088mm占硅石颗粒20～32wt％。
所述硅石细粉的SiO2含量≥98wt％；所述硅石细粉的粒径≤0.088mm。
所述硅微粉的SiO2含量≥92wt％；所述硅微粉的粒径≤0.6μm。
所述石灰乳的CaO≥60wt％。
所述氧化钇的Y2O3含量≥99wt％；所述氧化钇的粒径≤5μm。
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：
氢冶金反应温度低于铁的熔点，用高纯H2还原赤铁矿，经过800℃保温8h即可将铁的氧化物完全还原成为铁，同时产生大量的水蒸气。SiO2和H2反应如下：
SiO2+H2(g)＝SiO(g)+H2O(g)；
△Gθ＝-322.09T+488751。
上述反应在温度低于1517℃时吉布斯自由能变(△Gθ)为正数，表明该反应在1517℃以下不能自发进行。可以看出，氢冶金天然气基竖炉用硅砖的主要成分SiO2在氢冶金过程中具有良好的化学稳定性。
本发明以石灰乳为矿化剂，同时引入稀土氧化物Y2O3，氢冶金天然气基竖炉用硅砖在高温烧成过程中，Y2O3和石灰乳引入的CaO、硅石以及硅微粉中的SiO2反应生成Ca3Y2Si3O12结合相，Ca3Y2Si3O12结合相在高温H2-H2O混合气体中具有优异的化学稳定性，提高了氢冶金天然气基竖炉用硅砖的高温力学性能，延长使用寿命。
本发明制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa下的荷重软化温度为1670～1705℃；常温耐压强度为60～110MPa；经过900℃下的H2-H2O混合气体腐蚀10h后，耐压强度为50～80MPa。
因此，本发明制备的氢冶金天然气基竖炉用硅砖具有荷重软化点高、强度大、抗H2-H2O气体腐蚀性能强和使用寿命长的特点，适用于采用H2或H2+CO混合气为还原剂的氢冶金天然气基竖炉制铁。
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。
为避免重复，先将本具体实施方式所采用的物料统一描述如下，实施例中不再赘述：
所述硅石颗粒的SiO2含量≥98wt％；所述硅石颗粒的级配是：粒径小于5mm且大于等于3mm占硅石颗粒20～30wt％，粒径小于3mm且大于等于1mm占硅石颗粒40～55wt％，粒径小于1mm且大于等于0.088mm占硅石颗粒20～32wt％。
所述硅石细粉的SiO2含量≥98wt％；所述硅石细粉的粒径≤0.088mm。
所述硅微粉的SiO2含量≥92wt％；所述硅微粉的粒径≤0.6μm。
所述石灰乳的CaO≥60wt％。
所述氧化钇的Y2O3含量≥99wt％；所述氧化钇的粒径≤5μm。
实施例1
一种氢冶金天然气基竖炉用硅砖及其制备方法。本实施例所述制备方法是：
以55～60wt％的硅石颗粒、25～30wt％的硅石细粉、5～7wt％的硅微粉、4～6wt％的石灰乳和4～6wt％的氧化钇为原料，混合，再外加所述原料1～3wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以22～30℃/h的速率升温至1350～1390℃，保温11～12h，制得氢冶金天然气基竖炉用硅砖。
本实施例制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa条件下的荷重软化温度为1680～1705℃；常温耐压强度为95～110MPa；经过900℃条件下的H2-H2O混合气体腐蚀10h，耐压强度为65～80MPa。
实施例2
一种氢冶金天然气基竖炉用硅砖及其制备方法。本实施例所述制备方法是：
以59～65wt％的硅石颗粒、20～26wt％的硅石细粉、4～6wt％的硅微粉、3～5.5wt％的石灰乳和3.5～6wt％的氧化钇为原料，混合，再外加所述原料2～4wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以15～23℃/h的速率升温至1370～1410℃，保温9～11h，制得氢冶金天然气基竖炉用硅砖。
本实施例制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa条件下的荷重软化温度为1684～1700℃；常温耐压强度为90～104MPa；经过900℃条件下的H2-H2O混合气体腐蚀10h，耐压强度为59～78MPa。
实施例3
一种氢冶金天然气基竖炉用硅砖及其制备方法。本实施例所述制备方法是：
以64～71wt％的硅石颗粒、18～23wt％的硅石细粉、3～5.5wt％的硅微粉、2.5～5wt％的石灰乳和2～5wt％的氧化钇为原料，混合，再外加所述原料3～5wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以28～38℃/h的速率升温至1390～1430℃，保温8～10h，制得氢冶金天然气基竖炉用硅砖。
本实施例制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa条件下的荷重软化温度为1688～1672℃；常温耐压强度为68～95MPa；经过900℃条件下的H2-H2O混合气体腐蚀10h，耐压强度为57～71MPa。
实施例4
一种氢冶金天然气基竖炉用硅砖及其制备方法。本实施例所述制备方法是：
以70～75wt％的硅石颗粒、16～19wt％的硅石细粉、3～5wt％的硅微粉、2～4wt％的石灰乳和1～4wt％的氧化钇为原料，混合，再外加所述原料2～4wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以37～45℃/h的速率升温至1410～1450℃，保温7～11h，制得氢冶金天然气基竖炉用硅砖。
本实施例制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa条件下的荷重软化温度为1670～1690℃；常温耐压强度为60～88MPa；经过900℃条件下的H2-H2O混合气体腐蚀10h，耐压强度为50～75MPa。
本具体实施方式与现有技术相比具有如下积极效果：
氢冶金反应温度低于铁的熔点，用高纯H2还原赤铁矿，经过800℃保温8h即可将铁的氧化物完全还原成为铁，同时产生大量的水蒸气。SiO2和H2反应如下：
SiO2+H2(g)＝SiO(g)+H2O(g)；
△Gθ＝-322.09T+488751。
上述反应在温度低于1517℃时吉布斯自由能变(△Gθ)为正数，表明该反应在1517℃以下不能自发进行。可以看出，氢冶金天然气基竖炉用硅砖的主要成分SiO2在氢冶金过程中具有良好的化学稳定性。
本具体实施方式以石灰乳为矿化剂，同时引入稀土氧化物Y2O3，氢冶金天然气基竖炉用硅砖在高温烧成过程中，Y2O3和石灰乳引入的CaO、硅石以及硅微粉中的SiO2反应生成Ca3Y2Si3O12结合相，Ca3Y2Si3O12结合相在高温H2-H2O混合气体中具有优异的化学稳定性，提高了氢冶金天然气基竖炉用硅砖的高温力学性能，延长使用寿命。
本具体实施方式制备的氢冶金天然气基竖炉用硅砖经过检测：0.2MPa下的荷重软化温度为1670～1705℃；常温耐压强度为60～110MPa；经过900℃下的H2-H2O混合气体腐蚀10h后，耐压强度为50～80MPa。
因此，本具体实施方式制备的氢冶金天然气基竖炉用硅砖具有荷重软化点高、强度大、抗H2-H2O气体腐蚀性能强和使用寿命长的特点，适用于采用H2或H2+CO混合气为还原剂的氢冶金天然气基竖炉制铁。

Claims (6)

1.一种氢冶金天然气基竖炉用硅砖的制备方法，其特征在于：以55～75wt％的硅石颗粒、16～30wt％的硅石细粉、3～7wt％的硅微粉、2～6wt％的石灰乳和1～6wt％的氧化钇为原料，混合，再外加所述原料1～5wt％的亚硫酸纸浆废液，混炼，压制成型，烘干；然后置于高温炉中，以15～45℃/h的速率升温至1350～1450℃，保温7～12h，制得氢冶金天然气基竖炉用硅砖；
所述硅石颗粒的SiO2含量≥98wt％；所述硅石颗粒的级配是：
粒径小于5mm且大于等于3mm占硅石颗粒20～30wt％，
粒径小于3mm且大于等于1mm占硅石颗粒40～55wt％，
粒径小于1mm且大于等于0.088mm占硅石颗粒20～32wt％。
2.根据权利要求1所述的氢冶金天然气基竖炉用硅砖的制备方法，其特征在于所述硅石细粉的SiO2含量≥98wt％，所述硅石细粉的粒径≤0.088mm。
3.根据权利要求1所述的氢冶金天然气基竖炉用硅砖的制备方法，其特征在于所述硅微粉的SiO2含量≥92wt％，所述硅微粉的粒径≤0.6μm。
4.根据权利要求1所述的氢冶金天然气基竖炉用硅砖的制备方法，其特征在于所述石灰乳的CaO≥60wt％。
5.根据权利要求1所述的氢冶金天然气基竖炉用硅砖的制备方法，其特征在于所述氧化钇的Y2O3含量≥99wt％，所述氧化钇的粒径≤5μm。
6.一种氢冶金天然气基竖炉用硅砖，其特征在于所述氢冶金天然气基竖炉用硅砖是根据权利要求1～5项中任一项所述的氢冶金天然气基竖炉用硅砖及其制备方法所制备的氢冶金天然气基竖炉用硅砖。
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