CN116396062A - 一种含盐废水焚烧炉用尖晶石复合铬刚玉砖及其制备方法 - Google Patents
一种含盐废水焚烧炉用尖晶石复合铬刚玉砖及其制备方法 Download PDFInfo
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 46
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- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 7
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Abstract
一种含盐废水焚烧炉用尖晶石复合铬刚玉砖及其制备方法，按重量份各组分为：粒径≤3mm的电熔铬刚玉：其中w(Al2O3)+w(Cr2O3)≥93%，40‑50份；粒径≤3mm的电熔白刚玉，其中w(Al2O3)≥99%，30‑45份；粒径≤8μm的氧化铬微粉，其中w(Cr2O3)≥99%，3‑12份；粒径≤8μm的镁铝尖晶石微粉，2‑12份；粒径≤4μm的氧化铝微粉，其中w(Al2O3)≥99%，1‑8份；结合剂：磷酸二氢铝，2‑5份；经混料、成型、干燥、烧成步骤制成，本申请通过镁铝尖晶石与基质中的氧化铬原位形成了Mg(Al1‑xCrx)2O4复合尖晶石和多元固溶体，使其具备高耐火度、高机械强度和优异的抗侵蚀性，尤其针对碱金属盐等具备优秀的抗侵蚀性。
Description
技术领域
本发明涉及耐火材料技术领域，尤其是涉及一种含盐废水焚烧炉用尖晶石复合铬刚玉砖及其制备方法。
背景技术
近年来，随着环保的要求的提高以及循环经济政策的推进，对化工行业含盐废水的处理越来越重视，焚烧法不仅能够将化工含盐废水处理至符合环保排放要求，且在焚烧处理化工含盐废水时能够回收利用部分资源，因此焚烧法成为了化工含盐废液无害化处理的最佳选择之一。
焚烧处理化工含盐废水的关键设备是焚烧炉，其工作衬里通常采用Al2O3-SiO2质耐火材料，然而现有的Al2O3-SiO2质耐火材料在高温服役过程中易受到碱金属盐严重侵蚀，造成损毁。耐火材料的损坏带来的成本提高不仅是由于购买和安装新的耐火炉衬，还会由于窑炉的停顿，降低生产效率，所以对于化工含盐废水焚烧炉而言，耐火材料是决定其长期稳定运行的关键，进而开发化工含盐废水焚烧炉用新型耐火材料势在必行。
现有的Al2O3-Cr2O3质耐火材料相较于Al2O3-SiO2质耐火材料耐火度、机械强度和抗侵蚀性有所提高，然而在化工含盐废水焚烧炉严酷的高温环境及碱金属盐尤其是碱金属盐（如硫酸钠等）的侵蚀条件下，Al2O3-Cr2O3质耐火材料的高温性能与抗侵蚀性仍需要进一步提升以满足焚烧炉需求。
发明内容
为了克服背景技术中的不足，本发明公开了一种含盐废水焚烧炉用尖晶石复合铬刚玉砖及其制备方法。
为实现上述发明目的，本发明采用如下技术方案：
一种含盐废水焚烧炉用尖晶石复合铬刚玉砖，按重量份各组分为：粒径≤3mm的电熔铬刚玉：其中w(Al2O3) + w(Cr2O3) ≥93%，40-50份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，30-45份；粒径≤8 μm的氧化铬微粉，其中w(Cr2O3)≥99%，3-12份；粒径≤8μm的镁铝尖晶石微粉，2-12份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%，1-8份；结合剂：磷酸二氢铝，2-5份。
制备方法如下，
混料：按配比称取各种原料，在混料机中混合均匀。
成型：混合后的料困料12~24h后，成型压力120-180MPa。
干燥：成型后生坯在干燥温度110~150℃下，干燥24h。
烧成：干燥后的样品在1500~1600℃高温炉中保温3-5h烧成。
优选的，所述含盐废水焚烧炉用尖晶石复合铬刚玉砖中的电熔铬刚玉为冶炼金属铬产生的铝铬渣经处理后所得，其中w(Al2O3) + w(Cr2O3) ≥93%，w(Cr2O3)≥12%。
由于采用如上所述的技术方案，本发明具有如下有益效果：
1. 采用冶炼金属铬产生的铝铬渣经处理后所得铬刚玉固溶体为原料，并且利用基质中添加较细的氧化铝微粉，在烧成过程中利用氧化铝微粉的高活性能够在较低的温度下与氧化铬微粉原位生成铬刚玉固溶体，减少了高温氧化铬的挥发，活化了晶格，也促进了材料的烧结，使材料的致密度增加，常温、高温强度提高；
2.采用镁铝尖晶石微粉部分替代基质中Cr2O3微粉，不仅减少了材料中氧化铬的含量，而且利用粒度较细的镁铝尖晶石微粉比表面积大、活性高的特点，在烧成过程中镁铝尖晶石与基质中的氧化铬原位形成了Mg(Al1-xCrx)2O4复合尖晶石和多元固溶体，复合尖晶石的生成会引起晶体结构缺陷，活化晶格，从而提高体系扩散传质速度，促进了材料的烧结，降低了烧结温度，材料显气孔率减少；同时也促进试样基质颗粒间结合强度增强，从而提高试样常温、高温强度，并且Mg(Al1-xCrx)2O4相较于Al2O3-Cr2O3更不易与碱金属反应，进一步抑制了六价铬的产生；
3.另外Mg(Al1-xCrx)2O4复合尖晶石的热膨胀系数相对于Al2O3-Cr2O3体系较小，而低热膨胀系数对抗热震性有利，从而提高了热震稳定性。原位生成的Mg(Al1-xCrx)2O4复合尖晶石和(Al1-xCrx)2O3不和碱金属盐反应，具有良好的抗碱金属盐侵蚀性；另一方面，原位Mg(Al1-xCrx)2O4复合尖晶石的生成，提高了基质内颗粒间结合程度，降低了气孔率，从而提高了抗含碱金属盐盐渣的侵蚀渗透性能；
4.由于材料基质中氧化铝微粉与镁铝尖晶石微粉的组合联动效果，在较低温度下实现了氧化铬与氧化铝及镁铝尖晶石的固溶，减少了高温氧化铬的挥发及六价铬的产生，所制备的尖晶石复合铬刚玉性能优于一般的铬刚玉砖，使焚烧炉内衬耐火材料寿命提高；
5. 本发明能够采用冶炼金属铬产生的铝铬渣经处理后所得铬刚玉固溶体为原料，实现了资源的循环利用。
附图说明
图1：侵蚀试样的扫描电镜（SEM）；
图2：实施例1、2和3的尖晶石复合铬刚玉砖用含碱金属盐盐渣侵蚀后坩埚截面图的照片；
图3为侵蚀试样中不同深度的Na元素相对含量（wt%）。
图中：（a）未加镁铝尖晶石的铬刚玉砖、（b）实施例1、（c）实施例2、（d）实施例3、（CPL）图像侵蚀渗透层、（UL）原砖层。
具体实施方式
一种化工含盐废水焚烧炉用尖晶石复合铬刚玉砖，按重量份各组分为：粒径≤3mm的电熔铬刚玉：其中w(Al2O3) + w(Cr2O3) ≥93%，40-50份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，30-45份；粒径≤8 μm的氧化铬微粉，其中w(Cr2O3)≥99%，3-12份；粒径≤8μm的镁铝尖晶石微粉，2-12份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%，1-8份；结合剂：磷酸二氢铝，2-5份。
将上述原料按要求配比混合，于混料机中混合均匀，混合好的料室温下困料12-24h，然后采用液压机压制成型为生坯，生坯干燥后于1500~1600℃高温炉中保温3-5h烧成。
实施例1
一种化工含盐废水焚烧炉用尖晶石复合铬刚玉砖，各组分重量份配比为：粒径≤3mm的电熔铬刚玉，50份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，32份；粒径≤8μm的氧化铬微粉，其中w(Cr2O3)≥99%， 12份；粒径≤8μm的镁铝尖晶石微粉：3份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%， 3份；结合剂：磷酸二氢铝，4份；
将上述原料按要求配比混合，与混料机中混合均匀，困料12h，用液压机压制成型，成型压力为150MPa，130℃干燥后生坯于1500℃高温炉中保温5h烧成。
实施例2
一种化工含盐废水焚烧炉用尖晶石复合铬刚玉砖，各组分重量份配比为：粒径≤3mm的电熔铬刚玉，40份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，41份；粒径≤8μm的氧化铬微粉，其中w(Cr2O3)≥99%， 9份；粒径≤8μm的镁铝尖晶石微粉：6份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%，4份；结合剂：磷酸二氢铝，3份；
将上述原料按要求配比混合，与混料机中混合均匀，困料18h，用液压机压制成型，成型压力为160MPa，100℃干燥后生坯于1550℃高温炉中保温4h烧成。
实施例3
一种化工含盐废水焚烧炉用尖晶石复合铬刚玉砖，各组分重量份配比为：粒径≤3mm的电熔铬刚玉，45份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，37份；粒径≤8μm的氧化铬微粉，其中w(Cr2O3)≥99%，6份；粒径≤8μm的镁铝尖晶石微粉：9份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%，3份；结合剂：磷酸二氢铝，3份；
将上述原料按要求配比混合，与混料机中混合均匀，困料24h，用液压机压制成型，成型压力为180MPa，在150℃干燥后生坯于1600℃高温炉中保温3h烧成。
实施例1～实施例3制得的尖晶石复合铬刚玉砖理化指标如表1所示：
表1：实施例1、2和3的尖晶石复合铬刚玉砖以及现有技术理化性能
结合附图，由图1能够看出，未加镁铝尖晶石的铬刚玉砖（a）和实施例1（b）试样都由侵蚀渗透层（CPL）和原砖层（UL）两部分组成，且侵蚀渗透层因原渣（碱金属盐）的侵蚀渗透变得较为致密，原砖层气孔率相对较高；随MgAl2O4的加入，试样的侵蚀渗透层深度由5.4mm降至3.5mm。
图2能够看出，实施例1（b）、实施例2（c）和实施例3（d）的材料采用静态坩埚法经1200 ℃，保温12h侵蚀实验，坩埚侵蚀后坩埚轮廓清晰完整，没有明显的侵蚀现象。
图3显示采用能谱仪（EDS）打点分析M0（未加镁铝尖晶石）和M2（实施例2）侵蚀试样中不同位置的Na元素分布，以此来表示渣在耐火材料中的渗透深度，由图3能够看出，实施例2相比对照组的侵蚀渗透层中钠元素含量较少，侵蚀深度较小，抗碱金属盐侵蚀性能较好。
本发明未详述部分为现有技术，对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明；因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内，不应将权利要求中的任何附图标记视为限制所涉及的权利要求。
Claims (7)
1.一种含盐废水焚烧炉用尖晶石复合铬刚玉砖，其特征是：按重量份各组分为：粒径≤3mm的电熔铬刚玉：其中w(Al2O3) + w(Cr2O3) ≥93%，40-50份；粒径≤3mm的电熔白刚玉，其中w(Al2O3) ≥99%，30-45份；粒径≤8 μm的氧化铬微粉，其中w(Cr2O3)≥99%，3-12份；粒径≤8 μm的镁铝尖晶石微粉，2-12份；粒径≤4 μm的氧化铝微粉，其中w(Al2O3) ≥99%，1-8份；结合剂：磷酸二氢铝，2-5份。
2.如权利要求1所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖，其特征是：所述一种含盐废水焚烧炉用尖晶石复合铬刚玉砖的制备方法为，
混料：按配比称取各种原料，在混料机中混合均匀；
成型：混合后的物料困料12-24h后，采用液压机压制成型为生坯，120-180Mpa压制成型；
干燥：成型后生坯在干燥温度110~150℃下进行干燥24h±1h；
烧成：干燥处理后的半成品经1500~1600℃高温炉中保温3-5h烧成，得到含盐废水焚烧炉用尖晶石复合铬刚玉砖。
3.如权利要求1所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖，其特征是：所述含盐废水焚烧炉用尖晶石复合铬刚玉砖中的电熔铬刚玉为冶炼金属铬产生的铝铬渣经处理后所得。
4.如权利要求1所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖，其特征是：所述含盐废水焚烧炉用尖晶石复合铬刚玉砖中的电熔铬刚玉w(Al2O3) + w(Cr2O3) ≥93%，w(Cr2O3)≥12%。
5.如权利要求2所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖的制备方法，其特征是：所述困料时间为12h，成型压力为150MPa，130℃干燥后生坯于1500℃高温炉中保温5h烧成。
6.如权利要求2所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖的制备方法，其特征是：所述困料时间为18h，成型压力为160MPa，100℃干燥后生坯于1550℃高温炉中保温4h烧成。
7.如权利要求2所述的一种含盐废水焚烧炉用尖晶石复合铬刚玉砖的制备方法，其特征是：所述困料时间为24h，成型压力为180MPa，150℃干燥后生坯于1600℃高温炉中保温3h烧成。
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