CN111704471B - 一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法 - Google Patents

一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法 Download PDF

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CN111704471B
CN111704471B CN202010561314.4A CN202010561314A CN111704471B CN 111704471 B CN111704471 B CN 111704471B CN 202010561314 A CN202010561314 A CN 202010561314A CN 111704471 B CN111704471 B CN 111704471B
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左亮珠
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Abstract

本发明公开了一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法，主要原料包括工业废料(多晶硅切割废料和废电极)，辅料为硅溶胶、沥青、α‑Al2O3微粉和催化剂等，其中将多晶硅切割废料粉磨筛分成不同粒度级配，废电极磨成颗粒，混合浇注，低温硬化成型。本发明制备的浇注料硬度好，热导率高，机械性能强，相比于一般的碳砖材料和现有的浇注料，本发明利用高炉炉底炉缸的高温环境，将工业废料原位合成碳化硅，成本低、工艺简单、性能优良，适合应用于高炉炉底、炉缸等恶劣的工作环境中。

Description

一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的 方法
技术领域
本发明涉及一种工业废料增值利用途径和制备方法，具体为一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法，属于无机非金属材料的合成技术领域。
背景技术
近年来，我国多晶硅在太阳能电池中的使用量越来越大，而在太阳能电池生产过程中，切割工艺是必不可少的流程之一，无论是传统的砂浆线锯切割技术还是新兴的金刚线切割技术，在切割过程中都会产生大量多晶硅切割废料，经年累积堆存，既是对环境的污染又是对资源的浪费。这些废料往往含有大量的金属硅、二氧化硅和磨具材料(氧化铁或者碳)等，是制备碳化硅耐火材料的理想原料。
同时，随着生态文明建设的推进，钢铁工业受到环保政策的影响，频繁的技术整改和季度限产导致高炉长期非持续性运作，炉底侵蚀和炉缸烧穿的风险大大增加，高炉寿命明显缩短，成为困扰我国钢铁冶炼行业的技术难题。碳砖作为传统的炉底、炉缸耐火材料，利用了石墨的高导热性、低热膨胀性，以及与炉渣的不润湿性。频繁的停炉点火导致的热应力不稳定和炉震加速了碳砖膨胀开裂与粉化，严重加剧了铁水对碳砖的侵蚀。塑性耐火浇筑料是一种浇筑整体成型的新型高炉炉底、炉缸耐火材料，相比于导热性较差和易脆裂粉化的碳砖，耐火浇筑料具有更好的高温导热性、抗震性和高温下的耐压强度。
因此，本发明以多晶硅产业产生的工业废料和废电机颗粒等工业固废为原材料，利用高炉生产工艺的热源，原位制备合成高炉炉底炉缸用耐火浇注料，制备出的耐火浇筑料具有高导热性，抗热震性好，高温耐压强度优异，并且原料为工业废料，来源广，成本低，制备工艺简单，优势非常明显。
发明内容
本发明的目的就在于开发一种利用工业废料原位制备高炉炉底炉缸浇注料的工艺方法，实现工业废料的高值利用。
本发明通过以下技术方案来实现上述目的，一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法，所述制备方法包括如下步骤：
(1)原料选取，主要原料：多晶硅切割废料作为硅源，废电极作为碳源，硅溶胶、沥青、α-Al2O3微粉和催化剂作为辅料。
(2)浇注料的制备：原料重量组份为，多晶硅切割废料50％-60％，废电极15-25％，沥青10-15％，硅溶胶3-8％，α-Al2O3微粉3-8％，催化剂1-3％。
(3)所选用的多晶硅切割废料为光伏产业加工废料，主要成分为金属硅、二氧化硅、碳化硅和少量铁氧化物等。将多晶硅切割废料粉磨筛分成不同粒度级配(0-48μm，48-150μm以及150-1000μm)；
(4)所选用的废电极为工业废旧石墨电极其中固定碳大于70％，废电极磨成颗粒(150-1000μm)；
(5)所选用的硅溶胶和沥青属于中低温下体系的粘结剂，且可以分别作为硅元素和碳元素来源。
(6)所述的催化剂包括三氧化二铁、硼砂(或氧化硼)、硫酸镍(或氧化镍)等。
(7)多晶硅切割废料、废电极颗粒、沥青、硅溶胶、α-Al2O3微粉、催化剂放进搅拌机内室温混合2分钟，待混合完成后进行浇注，浇筑完成后放置12-24小时即可完成低温下硬化成型。
优选的，多晶硅切割废料的粒度级配为粒度0-48μm，40％；粒度48-150μm，30％；粒度150-1000μm，30％。
所述废电极为工业废旧石墨电极，其中固定碳大于70％。废电极磨成颗粒150-1000μm。
所述硅溶胶和沥青属于中低温下体系的粘结剂，且可以分别作为硅元素和碳元素来源。
所述催化剂为三氧化二铁、硼砂、氧化硼、硫酸镍、氧化镍中的一种或多种。
α-Al2O3微粉的粒度不大于10μm。
本发明的沥青使用中间相沥青。沥青用于耐火材料粘结剂也是比较普遍的，沥青的作用分为物理粘结和炭化过程，温度较低的时候属于物理粘结，作用类似于硅溶胶。随着温度升高，沥青会发生炭化、石墨化转化，形成强度更高的化学粘结效应。表中的数据是研究对比了酚醛树脂和中间相沥青分别作为耐火材料粘结剂时，随着温度升高对材料强度的影响。
不同温度下两种黏结剂型块的耐压强度
Figure GDA0002583008170000031
之所以提到烘炉温度(300℃以上)主要因为沥青的炭化转化开始温度在300℃左右，这个阶段沥青对强度的贡献会区别于硅凝胶，慢慢提升。
本发明的有益效果是：原料经过混合浇筑后，首先在低温下成型，此时起作用的粘结剂主要是硅溶胶和沥青，而后随着烘炉操作，温度升高沥青开始炭化，对于强度的贡献升高，进一步增加强度，而后在生产过程中温度达到1500-1550℃后多晶硅切割料与废电极反应原位生成碳化硅，达到最终的性能要求。该制备的炉底炉缸高导热浇注料高温机械性能良好，导热性好，适合应用于高炉炉底、炉缸等恶劣工作环境中，且原料来源为工业废料，既解决了高炉运行中现存的问题，又实现了工业废料的高值化利用，经济和生态效益显著。
具体实施方式
下面将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。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一：
一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料，所述制备方法如下：
所述制备方法包括如下步骤：
(1)原料选取，主要原料：多晶硅切割废料，废电极，硅溶胶、沥青、α-Al2O3微粉和催化剂三氧化二铁；
(2)将多晶硅切割废料粉磨筛分成不同粒度级配(0-48μm40％，48-150μm30％以及150-1000μm30％)，废电极磨成颗粒(150-1000μm)；α-Al2O3微粉的粒度不大于10μm；
(3)主要原料中分别取多晶硅切割废料50％，废电极20％，沥青13％，硅溶胶5％，α-Al2O3微粉8％，三氧化二铁3％；
(4)多晶硅切割废料、废电极颗粒、沥青、硅溶胶、α-Al2O3微粉、催化剂放进搅拌机内室温混合2分钟，待混合完成后进行浇注，浇筑完成后放置24小时即可完成低温下硬化成型；
上述制备方法碳化硅浇注料导热系数为21W/(m*K)，抗压强度为43MPa，耐磨性好，机械性能强。
实施例二：
一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料，所述制备方法如下：
所述制备方法包括如下步骤：
(1)原料选取，主要原料：多晶硅切割废料，废电极，硅溶胶、沥青、α-Al2O3微粉和催化剂三氧化二铁；
(2)将多晶硅切割废料粉磨筛分成不同粒度级配(0-48μm40％，48-150μm30％以及150-1000μm30％)，废电极磨成颗粒(150-1000μm)；α-Al2O3微粉的粒度不大于10μm。
(3)主要原料中分别取多晶硅切割废料55％，废电极18％，沥青12％，硅溶胶4％，α-Al2O3微粉7％，氧化硼4％；
(4)多晶硅切割废料、废电极颗粒、沥青、硅溶胶、α-Al2O3微粉、催化剂放进搅拌机内室温混合2分钟，待混合完成后进行浇注，浇筑完成后放置24小时即可完成低温下硬化成型；
上述制备方法碳化硅浇注料导热系数为24W/(m*K)，抗压强度为40MPa，耐磨性好，机械性能强。
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。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。

Claims (4)

1.一种利用工业废料原位制备高炉炉底炉缸用耐火浇注料的方法，其特征在于，所述方法包括如下步骤：
(1)原料选取：多晶硅切割废料作为硅源，废电极作为碳源，硅溶胶、沥青、α-Al2O3微粉和催化剂作为辅料；所述的多晶硅切割废料为光伏产业加工废料，主要成分为金属硅、二氧化硅、碳化硅和少量铁氧化物；所述废电极为工业废旧石墨电极，其中固定碳大于70％；
(2)浇注料的制备：原料重量组份为，多晶硅切割废料50％-60％，废电极15-25％，沥青10-15％，硅溶胶3-8％，α-Al2O3微粉3-8％，催化剂1-3％；所述催化剂为三氧化二铁、硼砂、氧化硼、硫酸镍、氧化镍中的一种或多种；所述硅溶胶和沥青属于中低温下体系的粘结剂，也分别作为硅元素和碳元素来源；
(3)将所述多晶硅切割废料粉磨筛分成不同粒度级配；
(4)将所述废电极磨成颗粒；
(5)将所述多晶硅切割废料、废电极颗粒、沥青、硅溶胶、α-Al2O3微粉和催化剂放进搅拌机内室温混合2分钟，待混合完成后进行浇注，浇注完成后放置12-24小时即可完成低温下硬化成型；
所述原位制备是指利用高炉生产过程中利用炉缸位置1500-1550℃的高温环境在催化剂的存在下，促使废电极中的石墨与多晶硅切割废料中的金属硅或者二氧化硅反应生产碳化硅晶体，原位烧成炉缸碳化硅耐火材料。
2.根据权利要求1所述的方法，其特征在于：步骤(3)中，所述多晶硅切割废料的粒度级配为粒度0-48μm，40％；粒度48-150μm，30％；粒度150-1000μm，30％。
3.根据权利要求1所述的方法，其特征在于：在室温下先将原料混匀2分钟，混合均匀后进行浇注，浇注后经12-24小时低温下硬化成型，沥青的胶凝性则体现在烘炉阶段300℃以上，进一步增加浇注料的强度。
4.根据权利要求1所述的方法，其特征在于：α-Al2O3微粉的粒度不大于10μm。
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